Khảo sát thành phần hóa học của hoa cây sơn cúc hai hoa wedelia biflora (l.) dc, họ cúc (asteraceae)

Mục lục Danh mục các ký hiệu và từ viết tắt Danh mục các bảng biểu, sơ đồ, hình ảnh Mở đầu Chương 1. TỔNG QUAN .1 1.1. Đặc tính thực vật của cây .1 1.1.1. Cây sơn cúc hai hoa . .1 1.1.2. Cây sơn cúc nhám . .1 1.1.3. Cây sơn cúc bò . 2 1.1.4. Cây sơn cúc ba thùy . 2 1.1.5. Cây Wedelia paludosa 2 1.1.6. Cây sài đất 2 1.1.7. Cây lỗ địa cúc .3 1.2. Thành phần hóa học . 6 1.2.1. Cây sơn cúc hai hoa . .6 1.2.2. Cây sơn cúc nhám . .6 1.2.3. Cây sơn cúc bò . 6 1.2.4. Cây sơn cúc ba thùy . 6 1.2.5. Cây Wedelia paludosa 7 1.2.6. Cây sài đất 8 1.2.7. Cây lỗ địa cúc .8 1.3. Dược tính học . .13 1.3.1. Cây sơn cúc hai hoa . .13 1.3.2. Cây sơn cúc nhám . .14 1.3.3. Cây sơn cúc bò . 14 1.3.4. Cây sơn cúc ba thùy . 14 1.3.5. Cây Wedelia paludosa 14 1.3.6. Cây sài đất 15 1.3.7. Cây lỗ địa cúc .15 Chương 2. THỰC NGHIỆM 16 2.1. Hóa chất, thiết bị 16 2.1.1. Hóa chất 16 2.1.2. Thiết bị .16 2.2. Khảo sát nguyên liệu 17 2.2.1. Xử lý mẫu cây 17 2.2.2. Xác định độ ẩm .17 2.3. Điều chế các loại cao . .17 2.4. Ly trích và cô lập một số hợp chất hữu cơ từ hoa của cây sơn cúc hai hoa-Wedelia biflora (L.) DC 21 2.4.1. Sắc ký cột silica gel áp dụng trên tủa eter dầu hỏa của bảng 2.1 .21 2.4.2. Sắc ký cột silica gel áp dụng trên cao E2 của bảng 2.1 .21 2.4.3. Sắc ký cột silica gel áp dụng trên cao C2 của bảng 2.1 .21 2.4.4. Sắc ký cột silica gel áp dụng trên cao C4 của bảng 2.1 .22 2.4.5. Sắc ký cột trên phân đoạn tủa etyl acetat (TEA) của bảng 2.1 22 Chương 3. KẾT QUẢ VÀ THẢO LUẬN .26 3.1. Khảo sát cấu trúc hóa học của hợp chất WEDE.FE1 .26 3.2. Khảo sát cấu trúc hóa học của hợp chất WEDE.FE2 .27 3.3. Khảo sát cấu trúc hóa học của hợp chất WEDE.FE3 .30 3.4. Khảo sát cấu trúc hóa học của hợp chất WEDE.FC1 34 3.5. Khảo sát cấu trúc hóa học của hợp chất WEDE.FC2 35 3.6. Khảo sát cấu trúc hóa học của hợp chất WEDE.FC5 40 3.7. Khảo sát cấu trúc hóa học của hợp chất WEDE.FC3 46 3.8. Khảo sát cấu trúc hóa học của hợp chất WEDE.FC4 50 3.9. Khảo sát cấu trúc hóa học của hợp chất WEDE.FC6 54 3.10. Khảo sát cấu trúc hóa học của hợp chất WEDE.FACE1 .57 Chương 4. KẾT LUẬN .60 Tài liệu tham khảo Phụ lục

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501.0 2910 1 | 695.8 396 0 | | 107.0 2272 1 | 310.1 2062 1 | 502.4 2386 1 | 697.4 425 0 | | 108.4 149 0 | 311.2 18863 9 | 503.6 1539 1 | 698.2 1825 1 | | 109.8 728 0 | 312.2 6939 3 | 505.3 3853 2 | 699.3 1481 1 | | 110.6 2853 1 | 313.4 3777 2 | 506.3 1871 1 | 700.3 320 0 | | 111.9 415 0 | 314.3 3596 2 | 507.3 4862 2 | 701.4 54 0 | | 112.7 425 0 | 315.4 348 0 | 508.1 587 0 | 702.9 2367 1 | | 114.6 2596 1 | 316.5 328 0 | 509.5 2167 1 | 703.9 1482 1 | | 115.9 83 0 | 318.2 9739 5 | 510.5 3149 2 | 705.3 4035 2 | | 117.2 178 0 | 319.3 1682 1 | 511.5 2853 1 | 706.3 758 0 | | 118.6 159 0 | 320.9 2196 1 | 513.0 3006 1 | 707.4 3595 2 | | 119.4 63 0 | 322.0 434 0 | 513.8 416 0 | 708.2 1205 1 | | 120.3 481 0 | 322.9 1214 1 | 515.0 3453 2 | 709.0 319 0 | | 121.2 425 0 | 324.2 1785 1 | 516.1 4224 2 | 709.9 729 0 | | 122.8 443 0 | 325.5 720 0 | 517.1 186 0 | 711.2 13101 6 | | 124.1 2757 1 | 326.7 140 0 | 518.5 2129 1 | 712.4 8586 4 | | 125.1 767 0 | 327.4 2596 1 | 519.4 443 0 | 713.6 6672 3 | | 126.1 368 0 | 328.4 253 0 | 520.5 5843 3 | 715.2 180101 89 | | 128.3 453 0 | 329.4 1320 1 | 521.4 1805 1 | 716.2 103757 51 | | 129.6 910 0 | 330.3 35 0 | 522.7 2053 1 | 717.4 65710 32 | | 131.6 139 0 | 331.2 6739 3 | 523.5 2872 1 | 718.4 14700 7 | | 132.4 549 0 | 332.1 3625 2 | 525.2 8453 4 | 719.5 6586 3 | | 134.4 320 0 | 333.2 1492 1 | 526.1 1872 1 | 720.8 113 0 | | 135.6 434 0 | 334.8 501 0 | 527.0 3672 2 | 722.0 664 0 | | 137.6 273 0 | 336.3 83 0 | 528.2 1482 1 | 723.1 882 0 | | 138.9 7262 4 | 337.5 463 0 | 529.7 3977 2 | 724.1 2063 1 | | 139.9 217 0 | 338.7 445 0 | 530.9 4110 2 | 725.9 2302 1 | | 141.3 529 0 | 339.4 311 0 | 532.3 139 0 | 727.3 2.021e+6 999 | | 143.2 2119 1 | 340.3 319 0 | 533.2 1053 1 | 728.3 1.037e+6 513 | | 144.3 245 0 | 341.1 1872 1 | 534.2 758 0 | 729.3 956843 473 | | 145.1 1681 1 | 342.2 748 0 | 535.2 3805 2 | 730.4 328330 162 | Print Date: 20 Jun 2009 11:25:51 Scan 46 from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc5.xms - Page 3 Ion Int Norm Ion Int Norm Ion Int Norm Ion Int Norm | 146.0 510 0 | 343.3 2519 1 | 536.1 378 0 | 731.3 184405 91 | | 147.0 806 0 | 345.1 3225 2 | 536.9 3948 2 | 732.4 59567 29 | | 148.0 3119 2 | 346.4 3167 2 | 537.7 624 0 | 733.3 25167 12 | | 149.2 1748 1 | 347.4 653 0 | 538.9 2957 1 | 734.1 6453 3 | | 151.1 786 0 | 348.2 310 0 | 540.3 1853 1 | 735.1 1739 1 | | 152.4 224 0 | 349.4 196 0 | 541.1 4548 2 | 736.4 4977 2 | | 153.7 186 0 | 350.3 1634 1 | 542.1 1310 1 | 737.6 9100 4 | | 155.3 168 0 | 352.4 1178 1 | 543.5 1100 1 | 738.5 2082 1 | | 156.4 664 0 | 353.2 5957 3 | 544.3 1167 1 | 739.7 4148 2 | | 157.1 6043 3 | 354.1 3149 2 | 545.5 1957 1 | 740.4 235 0 | | 158.2 596 0 | 355.5 472 0 | 546.7 3196 2 | 741.5 6186 3 | | 159.0 2062 1 | 357.0 2862 1 | 549.3 4920 2 | 743.4 35814 18 | | 160.5 1901 1 | 358.3 339 0 | 550.1 407 0 | 744.6 12367 6 | | 162.0 425 0 | 359.0 292 0 | 551.1 3900 2 | 745.4 14748 7 | | 163.2 529 0 | 360.8 872 0 | 552.3 4233 2 | 746.4 6139 3 | | 165.2 2682 1 | 362.4 2539 1 | 553.2 2185 1 | 747.3 8749 4 | | 166.5 3235 2 | 363.4 177 0 | 554.5 4605 2 | 748.4 2005 1 | | 168.2 188 0 | 364.1 519 0 | 555.4 3549 2 | 749.7 7815 4 | | 169.5 1453 1 | 365.1 4796 2 | 556.3 1244 1 | 750.6 9443 5 | | 170.7 1196 1 | 366.2 958 0 | 557.1 1882 1 | 751.6 8690 4 | | 171.5 46 0 | 367.2 6167 3 | 557.9 329 0 | 752.7 5177 3 | | 172.7 129 0 | 368.3 2767 1 | 559.1 4339 2 | 753.7 2806 1 | | 174.0 1014 1 | 369.6 359 0 | 560.3 862 0 | 754.6 5738 3 | | 175.0 4968 2 | 371.1 2253 1 | 561.1 653 0 | 756.3 6634 3 | | 175.8 3196 2 | 373.0 2978 1 | 562.3 3091 2 | 757.5 2005 1 | | 176.9 7014 3 | 374.5 3919 2 | 564.4 292 0 | 758.4 3396 2 | | 178.3 2548 1 | 375.4 3148 2 | 565.2 2262 1 | 759.3 4948 2 | | 179.4 4834 2 | 376.4 1606 1 | 566.5 130 0 | 760.9 7196 4 | | 180.9 2405 1 | 377.4 300 0 | 567.6 292 0 | 762.3 358 0 | | 182.1 510 0 | 379.5 1681 1 | 568.5 1643 1 | 763.5 5100 3 | | 183.4 264 0 | 380.2 786 0 | 569.3 1863 1 | 764.6 3043 2 | | 184.5 121 0 | 381.3 11185 6 | 570.1 83 0 | 765.4 3463 2 | | 185.3 2310 1 | 382.8 6482 3 | 571.3 1167 1 | 766.3 3901 2 | | 186.5 300 0 | 384.0 2519 1 | 573.0 2310 1 | 767.4 3710 2 | | 188.3 139 0 | 385.3 1662 1 | 574.0 2596 1 | 768.3 3710 2 | | 190.8 8 0 | 387.3 1824 1 | 575.3 1739 1 | 769.5 5777 3 | | 191.6 244 0 | 389.2 5434 3 | 576.4 2262 1 | 770.4 4825 2 | | 192.8 3435 2 | 390.3 1549 1 | 577.4 1148 1 | 771.3 3225 2 | | 194.0 4739 2 | 391.1 8377 4 | 579.1 1863 1 | 772.6 3339 2 | | 195.3 653 0 | 392.6 1072 1 | 580.4 3225 2 | 773.4 7053 3 | | 196.4 27 0 | 393.4 2406 1 | 581.5 377 0 | 774.7 4310 2 | | 197.7 2520 1 | 394.9 1320 1 | 582.4 4406 2 | 775.9 3414 2 | | 198.6 2396 1 | 396.3 1063 1 | 584.0 3119 2 | 778.2 3339 2 | | 199.8 3739 2 | 397.3 557 0 | 585.1 2167 1 | 779.4 1748 1 | | 200.7 3243 2 | 398.1 2320 1 | 586.4 445 0 | 780.6 1282 1 | | 201.6 310 0 | 399.3 3386 2 | 587.6 415 0 | 781.3 4586 2 | | 202.7 310 0 | 400.4 2853 1 | 588.8 2986 1 | 782.1 1092 1 | | 204.5 339 0 | 401.2 4577 2 | 589.7 377 0 | 783.0 520 0 | | 205.8 2301 1 | 402.4 74 0 | 590.9 2471 1 | 784.1 85 0 | | 206.8 376 0 | 403.2 4282 2 | 591.9 103 0 | 785.2 28586 14 | | 208.0 27 0 | 404.8 273 0 | 593.5 321 0 | 786.4 15338 8 | | 209.1 367 0 | 406.1 1834 1 | 595.2 2615 1 | 787.5 15653 8 | | 210.4 46 0 | 407.0 472 0 | 596.3 82 0 | 788.2 6835 3 | | 211.2 2796 1 | 407.9 310 0 | 597.9 862 0 | 789.3 8082 4 | | 212.0 396 0 | 409.1 5415 3 | 598.7 2291 1 | 790.0 2739 1 | | 212.8 54 0 | 410.2 3425 2 | 599.8 1596 1 | 791.2 586 0 | Print Date: 20 Jun 2009 11:25:51 Scan 46 from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc5.xms - Page 4 Ion Int Norm Ion Int Norm Ion Int Norm Ion Int Norm | 214.3 378 0 | 411.0 1700 1 | 601.6 405 0 | 792.7 424 0 | | 215.1 1110 1 | 412.2 2672 1 | 602.3 2777 1 | 793.6 2663 1 | | 216.9 605 0 | 413.1 9729 5 | 603.7 2015 1 | 794.3 2862 1 | | 218.1 1253 1 | 413.8 1472 1 | 604.8 3263 2 | 795.5 225 0 | | 219.3 321 0 | 415.2 463 0 | 605.9 1359 1 | 796.2 490 0 | | 220.6 64 0 | 416.1 1177 1 | 607.3 739 0 | 797.5 271 0 | | 222.2 2014 1 | 416.9 414 0 | 608.2 1033 1 | 798.8 377 0 | | 223.1 329 0 | 417.9 2348 1 | 609.2 1034 1 | 799.8 319 0 | | 224.8 996 0 | 419.2 6101 3 | 610.5 273 0 | 801.0 8367 4 | | 226.3 3625 2 | 420.3 3939 2 | 611.9 1082 1 | 802.5 3339 2 | | 227.1 6757 3 | 421.3 614 0 | 613.0 1882 1 | 803.4 2034 1 | | 228.7 2396 1 | 422.6 539 0 | 614.1 2176 1 | 804.7 387 0 | | 230.0 310 0 | 423.5 74 0 | 615.8 1425 1 | 805.8 577 0 | | 230.8 2167 1 | 425.3 3929 2 | 617.5 2653 1 | 806.5 329 0 | | 232.1 359 0 | 426.5 273 0 | 618.6 425 0 | 807.3 939 0 | | 232.9 2596 1 | 427.6 367 0 | 619.9 198 0 | 808.2 425 0 | | 234.2 300 0 | 429.2 4263 2 | 621.2 1167 1 | 809.2 758 0 | | 235.2 644 0 | 430.8 825 0 | 622.5 2520 1 | 810.0 1585 1 | | 236.2 767 0 | 432.3 1967 1 | 623.2 92 0 | 811.2 882 0 | | 237.4 3758 2 | 433.6 207 0 | 624.1 5834 3 | 812.0 1406 1 | | 238.9 1035 1 | 434.9 1967 1 | 625.0 1511 1 | 813.9 682 0 | | 240.1 863 0 | 437.1 3843 2 | 626.3 82 0 | 815.2 6234 3 | | 242.0 871 0 | 438.0 3567 2 | 627.6 1596 1 | 816.3 5558 3 | | 242.8 2147 1 | 439.1 3367 2 | 629.1 3148 2 | 817.3 1158 1 | | 244.3 3758 2 | 439.9 3092 2 | 630.3 425 0 | 818.9 2129 1 | | 245.1 872 0 | 441.4 939 0 | 631.1 986 0 | 820.0 1596 1 | | 246.5 113 0 | 442.2 197 0 | 631.8 2538 1 | 821.2 463 0 | | 247.3 27 0 | 443.5 2414 1 | 633.2 3767 2 | 822.1 129 0 | | 248.3 777 0 | 444.5 2691 1 | 634.5 368 0 | ... ... | WEDE.FC5−MeOD−1H 9 8 7 6 5 4 3 2 1 0 ppm 2 . 0 4 5 2 . 0 6 0 2 . 0 6 3 2 . 0 7 5 2 . 0 7 7 2 . 1 2 2 2 . 1 2 5 2 . 1 3 7 2 . 1 4 0 2 . 1 4 9 2 . 1 5 2 2 . 1 5 5 2 . 1 6 6 3 . 2 4 1 3 . 2 5 5 3 . 2 6 8 3 . 3 2 4 3 . 3 2 7 3 . 3 3 0 3 . 3 3 3 3 . 3 3 7 3 . 6 8 4 3 . 7 0 0 3 . 7 0 4 3 . 7 1 3 3 . 7 2 0 3 . 7 2 4 3 . 7 3 7 3 . 8 0 3 3 . 8 0 9 4 . 0 6 4 4 . 0 7 7 4 . 2 7 2 4 . 2 7 9 4 . 2 9 3 4 . 2 9 9 4 . 4 5 7 4 . 4 6 5 4 . 4 7 3 4 . 4 8 1 4 . 5 3 4 4 . 6 9 3 4 . 7 0 0 4 . 7 1 4 4 . 7 2 1 4 . 7 5 0 4 . 7 5 7 4 . 7 7 7 4 . 8 1 9 4 . 9 0 5 4 . 9 1 4 4 . 9 1 9 4 . 9 3 5 5 . 5 2 6 5 . 5 3 2 5 . 6 6 3 5 . 0 0 6 1 . 2 3 9 8 . 2 6 4 4 . 7 8 5 3 . 6 1 2 9 . 9 4 4 2 . 6 7 6 7 . 6 1 1 1 . 2 9 4 2 . 4 6 5 1 . 0 0 1 0 . 9 5 6 0 . 8 1 7 1 . 1 4 9 1 . 2 5 8 1 . 1 3 0 0 . 9 4 1 0 . 8 9 5 1 . 0 0 0 1 . 9 9 1 1 . 2 0 5 1 . 2 1 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300008 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −3.00 dB P1 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 303.3 K DE 6.00 usec DW 50.000 usec RG 181 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT MeOD TD 65536 PULPROG zg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 9.23 Date_ 20090528 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111THU.WEDE.FC5 Current Data Parameters 4 3 3''' 3'''' 3''''' 2' 4' 1' 3'' 1'' 3' 5' 4'' 5'' 2'' 8 W E D E . F C 5− Me OD −1 H 1. 0 1. 1 1. 2 1. 3 1. 4 1. 5 1. 6 1. 7 1. 8 1. 9 2. 0 2. 1 2. 2 2. 3 p p m 0.984 0.988 0.997 1.002 1.011 1.017 1.024 1.030 1.100 1.109 1.114 1.123 1.178 1.183 1.195 1.209 1.218 1.231 1.250 1.263 1.280 1.293 1.310 1.922 1.924 1.927 1.934 1.937 1.939 1.997 2.000 2.009 2.011 2.015 2.019 2.023 2.033 2.036 2.039 2.042 2.045 2.060 2.063 2.075 2.077 2.122 2.125 2.137 2.140 2.149 2.152 2.155 5.006 1.239 8.264 4.785 3.612 9.944 2.676 7.611 7 4' '' 4' '''5 ''' 5' ''' 4' '''' 5' '''' 6' ' 6' 9 10 WEDE.FC5−MeOD−C13CPD 200 180 160 140 120 100 80 60 40 20 0 ppm 1 5 . 9 0 1 1 6 . 0 6 1 1 6 . 4 1 1 1 6 . 4 4 5 1 6 . 6 2 1 1 6 . 8 7 4 2 0 . 6 8 0 2 0 . 9 7 8 2 3 . 0 7 8 2 4 . 6 9 1 2 6 . 7 3 0 2 6 . 8 6 8 4 8 . 4 8 9 4 8 . 6 5 8 4 8 . 8 2 8 4 8 . 9 9 9 4 9 . 1 6 8 4 9 . 2 8 5 4 9 . 3 4 0 4 9 . 4 5 3 4 9 . 5 1 0 4 9 . 6 2 6 6 9 . 2 3 0 7 0 . 5 6 9 7 1 . 8 0 9 7 1 . 8 9 8 7 1 . 9 9 1 7 4 . 2 7 2 7 7 . 4 9 1 7 9 . 0 7 5 1 0 5 . 2 0 2 1 0 6 . 5 5 5 1 1 7 . 3 6 3 1 2 4 . 4 3 2 1 2 8 . 4 6 6 1 2 8 . 7 3 1 1 2 9 . 0 8 1 1 2 9 . 2 5 2 1 3 9 . 2 0 7 1 3 9 . 7 6 4 1 4 0 . 8 3 9 1 4 1 . 6 2 4 1 4 2 . 7 7 2 1 4 8 . 9 9 4 1 6 7 . 9 1 1 1 6 8 . 8 4 2 1 6 9 . 2 4 2 PC 1.00 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7576139 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 22.00 dB PL12 14.68 dB PL2 −3.00 dB PCPD2 88.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7703643 MHz PL1 −1.00 dB P1 10.50 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 304.0 K DE 6.00 usec DW 16.650 usec RG 8192 AQ 1.0912410 sec FIDRES 0.458222 Hz SWH 30030.029 Hz DS 2 NS 4096 SOLVENT MeOD TD 65536 PULPROG zgpg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 18.08 Date_ 20090602 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111THU.WEDE.FC5 Current Data Parameters 6 5 3 1'' 1' 8 9 5''' 5'''' W E D E . F C 5− Me OD −C 13 CP D 11 0 11 5 12 0 12 5 13 0 13 5 14 0 14 5 15 0 15 5 16 0 16 5 17 0 p p m 105.202 106.555 117.363 124.432 128.466 128.731 129.081 129.252 139.207 139.764 140.839 141.624 142.772 148.994 167.911 168.842 169.242 1' '''' 1' ''' 1' '' 6 13 '''' 2 3' '' 3' '''' 4 5 3 1' ' 1' W E D E . F C 5− Me OD −C 13 CP D 70 71 72 73 74 75 76 77 78 79 p p m 69.230 70.569 71.809 71.898 71.991 74.272 77.491 79.075 16 17 18 19 20 21 22 23 24 25 26 27 28 p p m 15.901 16.061 16.411 16.445 16.621 16.874 20.680 20.978 23.078 24.691 26.730 26.868 3' 3' ' 4' 4' ' 2' ' 8 10 9 5' '' 5' ''' 5' '''' 6 6' ' 7 WEDE.FC5−MeOD−C13CPD 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm DEPT90 DEPT135 C13CPD CH&CH3 CH2 &DEPT Phuï luïc 31: Phoå D E PTcuûa hôïp chaát W E D E .FC 5 6 5 3 1'' 1' 8 9 3' 3'' 4' ppm 1234567 ppm 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 WEDE.FC5−MeOD−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300001 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300012 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 31.250000 Hz SFO1 500.1323 MHz TD 160 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −3.00 dB P1 10.50 usec P0 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 303.2 K DE 6.00 usec DW 100.000 usec RG 322.5 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 16 SOLVENT MeOD TD 2048 PULPROG cosygpqf PROBHD 5 mm Multinucl INSTRUM av500 Time 22.38 Date_ 20090602 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111THU.WEDE.FC5 Current Data Parameters Phuï luïc 32: Phoå C O SY cuûa hôïp chaát W E D E .FC 5 4 3 3''' 3'''' 3''''' 2' 4' 1' 3'' 1'' 3' 5' 4'' 5'' 2'' 8 7 5''' 5'''' 5''''' 6'' 10 4 3 3''' 3''''' 2' 4' 1' 3'' 1'' 3' 5' 4'' 8 7 5''''' 6'' 10 3'''' p p m 1234567 p p m 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 W E D E . F C 5 − M e O D − H S Q C 4 3 3 ' ' ' 3 ' ' ' ' 3 ' ' ' ' ' 2 ' 4 ' 1 ' 3 ' ' 1 ' ' 3 ' 5 ' 4 ' ' 5 ' ' 2 ' ' 8 7 6 ' ' 1 0 9 1 0 8 2 ' ' 4 ' ' 4 ' 3 ' ' 3 ' 1 ' 1 ' ' 3 5 6 p p m 1 . 01 . 52 . 02 . 53 . 03 . 5 p p m 1 4 1 5 1 6 1 7 1 8 1 9 2 0 2 1 2 2 2 3 2 4 2 5 2 6 2 7 2 8 W E D E . F C 5 − M e O D − H S Q C 8 7 4 ' ' ' 5 ' ' ' 5 ' ' ' ' 5 ' ' ' ' ' 6 ' ' 6 ' 9 1 0 7 4 ' ' ' ' ' 4 ' ' ' 6 5 ' ' ' ' ' 5 ' ' ' 5 ' ' ' ' 9 1 0 8 P h u ï l u ï c 3 3 a : P h o å H S Q C c u û a h ô ï p c h a á t W E D E . F C 5 p p m 3 . 84 . 04 . 24 . 44 . 64 . 85 . 05 . 25 . 45 . 6 p p m 7 0 7 5 8 0 8 5 9 0 9 5 1 0 0 1 0 5 W E D E . F C 5 − M e O D − H S Q C 2 ' ' 4 ' ' 4 ' 3 ' ' 3 ' 1 ' 1 ' ' 2 ' 4 ' 1 ' 3 ' ' 1 ' ' 3 ' 5 ' 4 ' ' 5 ' ' 2 ' ' P h u ï l u ï c 3 3 b : P h o å H S Q C c u û a h ô ï p c h a á t W E D E . F C 5 p p m 1234567 p p m 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 W E D E . F C 5 − M e O D − H M B C 4 3 3 ' ' ' 3 ' ' ' ' 3 ' ' ' ' ' 2 ' 4 ' 1 ' 3 ' ' 1 ' ' 3 ' 5 ' 4 ' ' 8 7 1 0 6 ' ' 9 1 0 8 2 ' ' 4 ' ' 4 ' 3 ' ' 3 ' 1 ' 1 ' ' 3 5 6 p p m 3 . 54 . 04 . 55 . 05 . 56 . 06 . 57 . 0 p p m 7 0 7 5 8 0 8 5 9 0 9 5 1 0 0 1 0 5 1 1 0 1 1 5 1 2 0 1 2 5 1 3 0 1 3 5 1 4 0 1 4 5 1 5 0 1 5 5 1 6 0 1 6 5 1 7 0 W E D E . F C 5 − M e O D − H M B C 4 3 3 ' ' ' 3 ' ' ' ' 3 ' ' ' ' ' 2 ' 4 ' 1 ' 3 ' ' 1 ' ' 3 ' 5 ' 4 ' ' 8 2 ' ' 4 ' ' 4 ' 3 ' ' 3 ' 1 ' 1 ' ' 3 5 6 1 ' ' ' 1 ' ' ' ' 1 ' ' ' ' ' 1 2 4 P h u ï l u ï c 3 4 a : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F C 5 p p m 1 . 01 . 52 . 02 . 53 . 03 . 5 p p m 1 2 0 1 2 5 1 3 0 1 3 5 1 4 0 1 4 5 1 5 0 1 5 5 1 6 0 1 6 5 1 7 0 W E D E . F C 5 − M e O D − H M B C 8 7 4 ' ' ' 5 ' ' ' 5 ' ' ' ' 5 ' ' ' ' ' 6 ' ' 6 ' 9 1 0 3 5 4 2 1 6 1 ' ' ' 1 ' ' ' ' 1 ' ' ' ' ' P h u ï l u ï c 3 4 b : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F C 5 WEDE.FC3−CDCl3−1H 9 8 7 6 5 4 3 2 1 0 ppm 2 . 0 4 4 2 . 0 4 7 2 . 0 6 6 2 . 0 8 0 2 . 1 0 9 2 . 1 1 2 2 . 1 2 3 2 . 1 2 6 2 . 1 6 6 2 . 1 7 6 2 . 2 0 9 2 . 2 1 4 2 . 2 3 9 2 . 2 5 2 2 . 4 6 1 2 . 4 7 6 2 . 5 7 9 2 . 6 8 0 2 . 6 8 9 3 . 2 2 3 3 . 2 3 2 3 . 2 4 5 3 . 2 5 9 3 . 2 7 3 3 . 2 8 7 3 . 4 7 5 3 . 4 8 2 3 . 4 8 9 3 . 4 9 3 3 . 5 0 1 3 . 5 0 5 3 . 5 2 6 3 . 5 3 7 3 . 5 4 9 3 . 8 1 3 3 . 8 2 6 3 . 8 3 9 3 . 8 5 1 3 . 9 5 2 3 . 9 5 9 3 . 9 6 6 3 . 9 7 3 3 . 9 7 9 3 . 9 8 6 3 . 9 9 3 4 . 7 4 1 4 . 7 5 7 4 . 7 6 2 4 . 7 7 1 4 . 7 7 8 4 . 7 8 7 4 . 7 9 3 5 . 0 9 8 5 . 1 1 1 5 . 1 1 6 5 . 1 3 1 5 . 1 4 9 1 . 2 5 7 1 . 0 4 0 2 . 7 1 0 1 . 5 6 3 1 . 8 8 0 3 . 3 5 0 1 . 4 9 3 3 . 9 8 3 2 . 0 0 0 2 . 5 2 1 4 . 3 0 8 6 . 9 6 4 3 . 0 7 2 4 . 8 0 6 0 . 3 4 3 0 . 8 7 9 1 . 3 6 9 1 . 1 0 8 0 . 9 9 4 0 . 9 2 7 1 . 4 5 4 0 . 5 6 2 0 . 9 4 9 1 . 3 2 0 2 . 3 4 5 1 . 4 6 2 1 . 4 7 8 0 . 3 3 5 1 . 0 0 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300141 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −1.00 dB P1 7.80 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 300.4 K DE 6.00 usec DW 50.000 usec RG 71.8 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 14.39 Date_ 20090112 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FC3 Current Data Parameters 3 4 3'' 3''' 2' 4' 1' 3' 5' 8 WEDE.FC3−CDCl3−1H 9 8 7 6 5 4 3 2 1 0 ppm 2 . 0 4 4 2 . 0 4 7 2 . 0 6 6 2 . 0 8 0 2 . 1 0 9 2 . 1 1 2 2 . 1 2 3 2 . 1 2 6 2 . 1 6 6 2 . 1 7 6 2 . 2 0 9 2 . 2 1 4 2 . 2 3 9 2 . 2 5 2 2 . 4 6 1 2 . 4 7 6 2 . 5 7 9 2 . 6 8 0 2 . 6 8 9 3 . 2 2 3 3 . 2 3 2 3 . 2 4 5 3 . 2 5 9 3 . 2 7 3 3 . 2 8 7 3 . 4 7 5 3 . 4 8 2 3 . 4 8 9 3 . 4 9 3 3 . 5 0 1 3 . 5 0 5 3 . 5 2 6 3 . 5 3 7 3 . 5 4 9 3 . 8 1 3 3 . 8 2 6 3 . 8 3 9 3 . 8 5 1 3 . 9 5 2 3 . 9 5 9 3 . 9 6 6 3 . 9 7 3 3 . 9 7 9 3 . 9 8 6 3 . 9 9 3 4 . 7 4 1 4 . 7 5 7 4 . 7 6 2 4 . 7 7 1 4 . 7 7 8 4 . 7 8 7 4 . 7 9 3 5 . 0 9 8 5 . 1 1 1 5 . 1 1 6 5 . 1 3 1 5 . 1 4 9 1 . 2 5 7 1 . 0 4 0 2 . 7 1 0 1 . 5 6 3 1 . 8 8 0 3 . 3 5 0 1 . 4 9 3 3 . 9 8 3 2 . 0 0 0 2 . 5 2 1 4 . 3 0 8 6 . 9 6 4 3 . 0 7 2 4 . 8 0 6 0 . 3 4 3 0 . 8 7 9 1 . 3 6 9 1 . 1 0 8 0 . 9 9 4 0 . 9 2 7 1 . 4 5 4 0 . 5 6 2 0 . 9 4 9 1 . 3 2 0 2 . 3 4 5 1 . 4 6 2 1 . 4 7 8 0 . 3 3 5 1 . 0 0 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300141 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −1.00 dB P1 7.80 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 300.4 K DE 6.00 usec DW 50.000 usec RG 71.8 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 14.39 Date_ 20090112 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FC3 Current Data Parameters 3 4 3'' 3''' 2' 4' 1' 3' 5' 8 W E D E . F C 3− CD Cl 3− 1H 0. 8 0. 9 1. 0 1. 1 1. 2 1. 3 1. 4 1. 5 1. 6 1. 7 1. 8 1. 9 2. 0 2. 1 2. 2 2. 3 2. 4 p p m 0.875 0.880 0.890 0.925 0.933 0.938 0.946 0.986 1.000 1.017 1.031 1.078 1.091 1.103 1.139 1.154 1.166 1.183 1.197 1.216 1.221 1.230 1.235 1.256 1.271 1.283 1.403 1.415 1.426 1.437 1.606 1.857 1.860 1.882 1.885 1.889 1.903 1.938 1.970 1.984 1.986 2.006 2.009 2.014 2.031 2.034 2.037 2.040 2.044 2.047 2.066 2.080 2.109 2.112 2.123 2.126 2.166 2.176 2.209 2.214 2.239 2.252 1.257 1.040 2.710 1.563 1.880 3.350 1.493 3.983 2.000 2.521 4.308 6.964 3.072 4.806 0.3437 4' '' 5' ' 4' ' 5' '' 6' 9 10 WEDE.FC3−CDCl3−C13CPD 200 180 160 140 120 100 80 60 40 20 0 ppm 1 5 . 7 1 7 1 5 . 8 7 8 1 6 . 0 6 8 1 6 . 3 0 8 1 7 . 3 4 1 2 0 . 2 2 9 2 0 . 2 7 1 2 0 . 6 5 9 2 2 . 7 7 9 2 4 . 0 2 7 2 5 . 7 4 6 7 0 . 5 8 7 7 2 . 0 9 1 7 2 . 3 4 1 7 2 . 4 8 8 7 6 . 7 1 5 7 6 . 9 6 9 7 7 . 2 2 3 1 0 3 . 4 7 8 1 1 6 . 2 5 0 1 2 3 . 5 6 1 1 2 7 . 0 4 7 1 2 7 . 1 7 2 1 2 7 . 6 2 3 1 3 9 . 6 4 0 1 4 0 . 0 1 7 1 4 0 . 1 5 6 1 4 1 . 2 7 2 1 4 7 . 8 7 5 1 6 7 . 5 5 6 1 6 7 . 6 3 0 PC 1.40 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7577825 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 22.00 dB PL12 14.68 dB PL2 −3.00 dB PCPD2 88.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7703643 MHz PL1 −1.00 dB P1 10.50 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 0.0 K DE 6.00 usec DW 16.650 usec RG 8192 AQ 1.0912410 sec FIDRES 0.458222 Hz SWH 30030.029 Hz DS 2 NS 2048 SOLVENT CDCl3 TD 65536 PULPROG zgpg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 18.06 Date_ 20090430 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111WEDE.FC3 Current Data Parameters 1'' 1''' 1 5 3 6 4 1' 5' W E D E . F C 3− CD Cl 3− C1 3C PD 20 25 30 35 40 45 50 55 60 65 70 p p m15.769 15.930 16.120 16.360 17.393 20.281 20.323 20.711 22.831 24.079 25.798 70.639 72.143 72.393 72.540 5' '' 5' ' 7 9 10 8 5' 6' 2' 3' 4' WEDE.FC3−CDCl3−C13CPD 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm DEPT90 DEPT135 C13CPD CH&CH3 CH2 &DEPT Phuï luïc 37: Phoå D E PT cuûa hôïp chaát W E D E .FC 3 1'' 1''' 1 5 3 6 4 1' 5' 8 9 7 ppm 1234567 ppm 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 WEDE.FC3−CDCl3−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300131 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300130 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −3.00 dB P1 10.50 usec P0 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 0.0 K DE 6.00 usec DW 100.000 usec RG 228.1 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm Multinucl INSTRUM av500 Time 20.49 Date_ 20090430 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111WEDE.FC3 Current Data Parameters Phuï luïc 38: Phoå C O SY cuûa hôïp chaát W E D E .FC 3 4 3 3''3''' 2' 4' 1' 3' 5' 8 7 6' 9 10 10 9 6' 7 8 5'3' 1' 4'2' 3'' 3''' 3 4 p p m 12345678 p p m 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 W E D E . F C 3 − C D C l 3 − H S Q C 4 3 3 ' ' 3 ' ' ' 2 ' 4 ' 1 ' 3 ' 5 ' 8 7 6 ' 9 1 0 7 9 8 5 ' 1 ' 3 5 4 1 6 p p m 1 . 01 . 52 . 02 . 53 . 03 . 5 p p m 1 3 1 4 1 5 1 6 1 7 1 8 1 9 2 0 2 1 2 2 2 3 2 4 2 5 2 6 2 7 2 8 2 9 3 0 3 1 W E D E . F C 3 − C D C l 3 − H S Q C 8 7 4 ' ' ' 5 ' ' ' 6 ' 9 1 0 7 4 ' ' 6 ' 5 ' ' ' 5 ' ' 9 1 0 8 P h u ï l u ï c 3 9 a : P h o å H S Q C c u û a h ô ï p c h a á t W E D E . F C 3 p p m 12345678 p p m 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 1 8 0 W E D E . F C 3 − C D C l 3 − H M B C 4 3 3 ' ' 3 ' ' ' 2 ' 4 ' 1 ' 3 ' 5 ' 8 7 6 ' 9 1 0 7 9 8 5 ' 1 ' 3 5 4 1 6 1 ' '1 ' ' ' p p m 1 . 01 . 52 . 02 . 53 . 0 p p m 1 1 5 1 2 0 1 2 5 1 3 0 1 3 5 1 4 0 1 4 5 1 5 0 1 5 5 1 6 0 1 6 5 1 7 0 1 7 5 W E D E . F C 3 − C D C l 3 − H M B C 8 7 4 ' ' ' 5 ' ' ' 6 ' 9 1 0 3 5 4 1 6 1 ' ' 1 ' ' ' P h u ï l u ï c 4 0 a : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F C 3 p p m 1 . 01 . 52 . 02 . 53 . 0 p p m 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 6 0 6 5 7 0 7 5 8 0 8 5 W E D E . F C 3 − C D C l 3 − H M B C 8 7 4 ' ' ' 5 ' ' ' 6 ' 9 1 0 7 6 ' 9 8 5 ' 5 ' ' ' 5 ' ' 2 ' 3 ' 4 ' P h u ï l u ï c 4 0 b : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F C 3 Print Date: 20 Jun 2009 11:23:40 Scan 114 from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc4.xms 100 200 300 400 500 600 700 800 m/z 0% 25% 50% 75% 100% 353.3 49710 381.3 152493 382.3 23262 409.1 151373 410.2 34359 672.6 28913 686.5 188814 687.4 105017 702.5 54537 703.5 32611 736.6 28449 Spectrum 1A 1.194 min, Scan: 114, 50.0:1000.0>, RIC: 2.934e+6BP: 686.5 (188814=100%), wede-fc4.xms Spectrum from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc4.xms Scan No: 114, Time: 1.194 minutes No averaging. Not background corrected. Comment: 1.194 min. Scan: 114 50.0:1000.0> RIC: 2.934e+6 Pair Count: 785 MW: 0 Formula: None CAS No: None Acquired Range: 50.0 - 1000.0 m/z Method Description: ESI Scan 1 Channel Description: 50.0:1000.0> ESI;CID -;Det EDR;WI Q1 Cal; Scan Information: cp = 0.0 mTorr Precursor Mass Range: 50.0 - 1000.0 m/z Phuï luïc 41: Phoå M S cuûa hôïp chaát W E D E .FC 4 Print Date: 20 Jun 2009 11:23:40 Scan 114 from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc4.xms - Page 2 Ion Int Norm Ion Int Norm Ion Int Norm Ion Int Norm | 78.0 38 0 | 286.5 1430 8 | 481.4 1068 6 | 681.3 3462 18 | | 79.0 62 0 | 287.4 675 4 | 483.2 3304 17 | 682.9 3050 16 | | 80.9 3637 19 | 288.7 2381 13 | 484.8 1480 8 | 683.9 2674 14 | | 81.6 20 0 | 289.4 1886 10 | 485.6 5 0 | 685.2 16817 89 | | 83.0 6592 35 | 290.5 961 5 | 487.0 1692 9 | 686.5 188814 999 | | 83.9 12 0 | 291.5 3419 18 | 488.5 1986 11 | 687.4 105017 556 | | 84.9 40 0 | 292.8 660 3 | 489.5 7232 38 | 688.5 86012 455 | | 86.2 94 0 | 294.9 1566 8 | 490.7 991 5 | 689.5 52449 278 | | 87.2 22 0 | 295.8 617 3 | 491.5 16 0 | 690.4 26517 140 | | 88.0 3675 19 | 296.9 20 0 | 492.5 3292 17 | 691.7 6929 37 | | 89.3 3741 20 | 297.8 33 0 | 493.7 919 5 | 692.8 1435 8 | | 91.0 1480 8 | 299.1 1768 9 | 495.2 838 4 | 693.7 5816 31 | | 91.7 79 0 | 301.2 14830 78 | 496.4 2065 11 | 694.8 251 1 | | 93.1 5 0 | 302.3 2369 13 | 497.2 4132 22 | 695.8 37 0 | | 94.5 18 0 | 303.5 849 4 | 498.1 30 0 | 697.0 2511 13 | | 96.0 18 0 | 304.6 1129 6 | 498.8 3860 20 | 697.7 41 0 | | 96.7 15 0 | 305.3 14 0 | 500.1 3510 19 | 698.4 3325 18 | | 98.8 2141 11 | 306.8 72 0 | 501.0 24 0 | 699.4 8816 47 | | 100.0 73 0 | 308.1 2553 14 | 502.1 16 0 | 700.6 53041 281 | | 100.8 5 0 | 309.2 15295 81 | 503.1 2676 14 | 701.6 46989 249 | | 102.0 12 0 | 311.1 8842 47 | 504.1 29 0 | 702.5 54537 289 | | 104.1 103 1 | 312.0 3515 19 | 505.3 4562 24 | 703.5 32611 173 | | 105.1 5930 31 | 313.0 2493 13 | 506.3 42 0 | 704.7 3348 18 | | 105.9 54 0 | 314.3 14 0 | 507.4 1858 10 | 705.6 5216 28 | | 107.1 7086 37 | 315.2 754 4 | 508.8 3031 16 | 706.4 1280 7 | | 108.6 25 0 | 316.2 3678 19 | 510.1 1507 8 | 707.2 56 0 | | 109.9 28 0 | 317.0 3392 18 | 511.0 3542 19 | 708.2 5319 28 | | 111.6 59 0 | 318.3 917 5 | 512.2 2194 12 | 709.5 4557 24 | | 112.7 2635 14 | 319.0 326 2 | 513.1 11 0 | 710.5 2761 15 | | 114.2 779 4 | 319.9 32 0 | 514.9 1 0 | 712.1 2503 13 | | 115.8 63 0 | 320.7 4318 23 | 515.9 41 0 | 713.1 4855 26 | | 116.6 29 0 | 321.6 2384 13 | 517.7 2924 15 | 714.6 93373 494 | | 117.9 1726 9 | 322.5 4716 25 | 518.5 594 3 | 715.6 47300 250 | | 119.3 990 5 | 323.2 1394 7 | 519.4 1275 7 | 716.6 52947 280 | | 120.8 2724 14 | 323.9 33 0 | 520.8 4 0 | 717.7 27916 148 | | 121.9 53 0 | 325.1 7315 39 | 521.6 36 0 | 718.9 8628 46 | | 122.7 2507 13 | 325.9 14 0 | 522.5 1787 9 | 720.2 4826 26 | | 123.7 29 0 | 327.0 2288 12 | 523.6 39 0 | 721.4 2432 13 | | 125.0 1173 6 | 328.5 22 0 | 524.3 1074 6 | 722.2 3428 18 | | 126.4 8 0 | 329.4 10 0 | 525.4 2055 11 | 723.3 2836 15 | | 128.0 38 0 | 330.3 401 2 | 526.9 603 3 | 724.6 2791 15 | | 129.1 1000 5 | 331.4 6178 33 | 527.6 190 1 | 726.2 1299 7 | | 130.3 34 0 | 332.4 1969 10 | 528.4 417 2 | 727.2 19320 102 | | 131.3 4101 22 | 333.3 60 0 | 529.8 619 3 | 728.8 11115 59 | | 132.7 28 0 | 334.4 1745 9 | 531.0 17 0 | 729.7 9617 51 | | 134.0 24 0 | 335.4 20 0 | 531.8 5 0 | 730.4 20513 109 | | 135.1 50 0 | 336.1 2822 15 | 533.3 5548 29 | 731.4 11361 60 | | 136.5 4 0 | 337.8 14 0 | 534.1 3378 18 | 732.7 6415 34 | | 137.9 20 0 | 338.6 30 0 | 535.6 1124 6 | 733.8 1522 8 | | 138.7 6303 33 | 339.4 18 0 | 537.8 144 1 | 734.7 4966 26 | | 139.5 11 0 | 341.1 1650 9 | 539.3 4 0 | 736.6 28449 151 | | 140.3 2286 12 | 343.0 1384 7 | 540.5 468 2 | 737.6 15793 84 | | 141.2 3317 18 | 345.1 2286 12 | 541.3 787 4 | 738.5 8805 47 | | 142.3 11 0 | 346.9 1444 8 | 542.6 732 4 | 739.6 509 3 | | 143.4 1456 8 | 347.9 679 4 | 543.5 96 1 | 740.7 64 0 | | 144.2 849 4 | 349.3 676 4 | 544.7 951 5 | 741.7 222 1 | Print Date: 20 Jun 2009 11:23:40 Scan 114 from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc4.xms - Page 3 Ion Int Norm Ion Int Norm Ion Int Norm Ion Int Norm | 145.0 68 0 | 350.5 70 0 | 546.1 536 3 | 742.6 8432 45 | | 146.1 903 5 | 352.4 1426 8 | 546.9 628 3 | 744.0 7828 41 | | 147.1 1816 10 | 353.3 49710 263 | 547.6 1816 10 | 744.7 16224 86 | | 147.9 2728 14 | 354.3 10376 55 | 548.4 23 0 | 746.1 5932 31 | | 150.1 2134 11 | 355.2 2217 12 | 549.2 4165 22 | 747.0 12173 64 | | 150.9 20 0 | 356.9 799 4 | 550.4 4150 22 | 748.1 6464 34 | | 151.6 2115 11 | 358.0 2747 15 | 551.3 2444 13 | 748.8 1622 9 | | 153.6 2716 14 | 360.1 862 5 | 552.9 1420 8 | 749.5 41 0 | | 155.4 44 0 | 361.1 8669 46 | 554.4 1054 6 | 750.4 6162 33 | | 156.8 8311 44 | 362.7 1485 8 | 555.3 1519 8 | 751.9 2820 15 | | 157.9 1131 6 | 364.6 1853 10 | 556.3 24 0 | 752.6 2411 13 | | 159.0 3428 18 | 365.4 28 0 | 557.1 523 3 | 753.3 1357 7 | | 159.9 28 0 | 366.4 2488 13 | 558.2 53 0 | 754.4 986 5 | | 160.6 6375 34 | 367.3 4807 25 | 559.6 1810 10 | 755.5 1399 7 | | 162.0 332 2 | 368.6 3118 16 | 560.6 840 4 | 756.9 5 0 | | 163.7 30 0 | 369.4 5310 28 | 562.4 2256 12 | 758.5 2862 15 | | 164.8 20 0 | 370.2 730 4 | 563.3 7149 38 | 759.5 2049 11 | | 166.1 38 0 | 372.0 11 0 | 564.2 4065 22 | 760.5 3886 21 | | 168.6 72 0 | 372.8 1268 7 | 565.1 5 0 | 762.2 5016 27 | | 169.6 2188 12 | 373.6 599 3 | 567.0 1981 10 | 763.4 432 2 | | 170.9 79 0 | 374.8 3816 20 | 567.7 3631 19 | 764.1 191 1 | | 171.7 93 0 | 376.7 1548 8 | 569.7 24 0 | 764.9 440 2 | | 172.8 2178 12 | 380.1 2744 15 | 571.2 47 0 | 766.4 18 0 | | 173.8 8737 46 | 381.3 152493 807 | 572.7 2567 14 | 767.1 4 0 | | 174.8 13932 74 | 382.3 23262 123 | 574.1 2523 13 | 768.3 1751 9 | | 176.1 3086 16 | 383.1 9005 48 | 575.3 3031 16 | 769.6 1478 8 | | 177.0 11505 61 | 384.4 87 0 | 576.1 5266 28 | 770.7 1107 6 | | 177.9 94 0 | 385.4 2299 12 | 577.5 8581 45 | 771.9 3166 17 | | 178.8 5069 27 | 386.2 2547 13 | 578.7 1785 9 | 773.0 2697 14 | | 179.8 19 0 | 387.2 4329 23 | 579.7 33 0 | 774.7 3980 21 | | 181.2 2044 11 | 389.1 5837 31 | 581.1 411 2 | 775.5 3595 19 | | 182.1 33 0 | 390.4 7169 38 | 581.8 1191 6 | 777.2 630 3 | | 183.1 3016 16 | 391.7 959 5 | 582.7 460 2 | 779.1 17 0 | | 184.9 8 0 | 392.6 6299 33 | 583.8 50 0 | 780.4 3266 17 | | 185.8 56 0 | 393.5 5511 29 | 585.0 37 0 | 782.2 1038 5 | | 186.8 3169 17 | 394.8 1148 6 | 586.5 1733 9 | 783.2 2368 13 | | 187.5 14 0 | 395.6 2770 15 | 587.5 2351 12 | 784.4 1573 8 | | 188.9 1274 7 | 397.2 4905 26 | 589.0 1382 7 | 785.6 4048 21 | | 190.8 59 0 | 398.0 705 4 | 590.5 149 1 | 787.4 1644 9 | | 193.7 2010 11 | 399.4 699 4 | 591.2 6410 34 | 788.5 1049 6 | | 195.0 61 0 | 401.2 3141 17 | 592.0 5950 31 | 789.9 543 3 | | 195.8 6 0 | 402.4 1461 8 | 593.1 66 0 | 791.9 755 4 | | 197.1 4328 23 | 404.1 20 0 | 594.3 47 0 | 792.8 1 0 | | 198.9 5541 29 | 405.6 1596 8 | 595.6 860 5 | 794.7 663 4 | | 199.9 76 0 | 406.6 30 0 | 597.0 1 0 | 795.4 589 3 | | 200.9 919 5 | 407.6 1686 9 | 597.9 42 0 | 796.3 515 3 | | 202.5 4242 22 | 409.1 151373 801 | 600.2 524 3 | 797.6 619 3 | | 203.5 16 0 | 410.2 34359 182 | 601.1 2 0 | 798.5 1330 7 | | 204.8 84 0 | 411.0 16944 90 | 602.3 393 2 | 799.7 645 3 | | 205.9 13 0 | 411.9 3462 18 | 603.2 2462 13 | 800.7 81 0 | | 206.9 1893 10 | 413.1 17100 90 | 604.5 2249 12 | 801.5 280 1 | | 208.2 45 0 | 414.3 5714 30 | 606.3 1935 10 | 803.3 2370 13 | | 208.9 1579 8 | 415.4 4215 22 | 608.0 411 2 | 804.2 734 4 | | 210.1 93 0 | 417.1 1831 10 | 609.1 984 5 | 804.9 4 0 | | 211.1 79 0 | 418.1 2960 16 | 611.1 58 0 | 805.6 60 0 | | 212.2 44 0 | 419.0 4233 22 | 612.0 32 0 | 806.9 743 4 | Print Date: 20 Jun 2009 11:23:40 Scan 114 from e:\du lieu ft-ms\6-2009\20-6-09\wede-fc4.xms - Page 4 Ion Int Norm Ion Int Norm Ion Int Norm Ion Int Norm | 213.2 2016 11 | 420.2 5219 28 | 613.4 1209 6 | 808.3 731 4 | | 215.1 3499 19 | 421.1 4794 25 | 614.4 1761 9 | 809.1 2513 13 | | 217.2 1032 5 | 422.3 3791 20 | 616.1 1636 9 | 810.2 872 5 | | 219.9 2510 13 | 423.2 2095 11 | 617.2 11 0 | 811.9 26 0 | | 221.3 4104 22 | 424.2 835 4 | 619.1 4966 26 | 812.8 28 0 | | 222.9 2178 12 | 425.2 14907 79 | 620.5 1548 8 | 814.4 33 0 | | 224.6 1093 6 | 426.2 5410 29 | 621.8 1449 8 | 815.6 11 0 | | 225.6 283 1 | 427.1 2180 12 | 623.1 941 5 | 816.5 3636 19 | | 226.5 16 0 | 428.1 1132 6 | 624.8 29 0 | 818.2 807 4 | | 227.8 3100 16 | 429.1 1024 5 | 626.2 14 0 | 819.6 644 3 | | 229.0 2126 11 | 431.1 3250 17 | 627.7 49 0 | 821.4 924 5 | | 230.2 654 3 | 432.3 8263 44 | 629.9 723 4 | 823.1 785 4 | | 231.0 10419 55 | 433.3 1865 10 | 630.9 7 0 | 824.4 2216 12 | | 232.9 4054 21 | 434.3 1833 10 | 631.8 1101 6 | 825.9 28 0 | | 233.8 1234 7 | 435.3 5388 29 | 632.8 3114 16 | 826.9 30 0 | | 234.8 12 0 | 436.7 367 2 | 634.3 19 0 | 828.1 3 0 | | 235.9 1437 8 | 437.5 31 0 | 635.7 11 0 | 829.3 3810 20 | | 236.9 5072 27 | 438.8 1957 10 | 636.4 11 0 | 830.1 77 0 | | 237.9 51 0 | 439.5 1466 8 | 637.6 2791 15 | 831.6 37 0 | | 239.0 793 4 | 440.3 743 4 | 639.5 1294 7 | 832.6 1291 7 | | 239.9 1937 10 | 441.1 6466 34 | 640.6 1350 7 | 834.5 53 0 | | 241.5 97 1 | 442.6 5898 31 | 642.2 1938 10 | 836.1 2163 11 | | 243.1 2442 13 | 443.5 1105 6 | 643.6 166 1 | 838.0 1673 9 | | 244.0 2 0 | 444.3 1637 9 | 645.4 862 5 | 839.3 974 5 | | 244.8 2228 12 | 445.3 5813 31 | 646.5 3349 18 | 841.5 1019 5 | | 245.6 2 0 | 446.6 1733 9 | 647.4 5403 29 | 842.3 835 4 | | 247.1 519 3 | 447.5 15507 82 | 648.3 6118 32 | 843.4 43 0 | | 248.8 4 0 | 448.3 2104 11 | 649.6 3944 21 | 844.7 9 0 | | 249.9 3936 21 | 449.5 824 4 | 651.2 32 0 | 845.5 1074 6 | | 252.2 1751 9 | 450.4 299 2 | 652.3 820 4 | 846.8 47 0 | | 254.1 81 0 | 451.2 10 0 | 653.0 37 0 | 848.1 1086 6 | | 254.9 13417 71 | 454.4 2949 16 | 654.5 1141 6 | ... ... | | 257.1 3413 18 | WEDE.FC4−CDCl3&MeOD−1H 7 6 5 4 3 2 1 0 ppm 1 . 5 2 8 1 . 5 3 2 1 . 5 4 5 1 . 5 5 3 1 . 5 6 1 1 . 5 6 4 1 . 5 7 1 1 . 5 7 6 1 . 5 8 7 1 . 5 9 7 1 . 6 0 8 1 . 7 8 8 1 . 7 9 6 1 . 8 0 1 1 . 8 0 8 1 . 8 1 6 1 . 8 2 2 1 . 8 2 8 1 . 8 3 6 1 . 8 4 5 1 . 8 4 8 1 . 8 5 6 1 . 9 4 4 1 . 9 5 6 1 . 9 7 0 1 . 9 8 3 2 . 0 0 4 2 . 0 1 7 2 . 0 2 9 2 . 0 4 3 3 . 3 7 7 3 . 3 8 0 3 . 3 9 8 3 . 4 1 4 3 . 5 0 8 3 . 5 2 4 3 . 5 4 1 3 . 7 0 5 3 . 7 1 6 3 . 7 2 0 3 . 7 2 4 3 . 7 3 8 3 . 9 0 1 3 . 9 1 0 3 . 9 1 4 3 . 9 2 2 4 . 0 1 3 4 . 0 2 0 4 . 0 2 9 4 . 0 3 7 4 . 1 3 9 4 . 1 5 4 4 . 1 7 1 4 . 2 5 5 4 . 2 6 9 4 . 2 8 3 6 . 2 2 5 6 2 . 1 4 6 3 . 3 9 8 3 . 6 2 0 1 . 1 0 9 1 . 4 7 8 1 . 2 6 1 1 . 0 4 4 1 . 0 1 9 1 . 0 3 4 1 . 0 2 7 1 . 0 4 1 1 . 0 0 0 1 . 2 4 3 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1299705 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −3.00 dB P1 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 303.2 K DE 6.00 usec DW 50.000 usec RG 143.7 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 8.59 Date_ 20090528 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111THU_WEDE.FC4 Current Data Parameters 8 9 2 1 2' 3 4 1 7 10 19 27' 3' 3' 5 6 4' WEDE.FC4−CDCl3&MeOD−C13CPD 180 160 140 120 100 80 60 40 20 0 ppm 2 2 . 7 5 8 2 5 . 3 6 5 2 5 . 8 3 3 2 5 . 8 7 9 2 9 . 2 9 5 2 9 . 4 2 1 2 9 . 4 3 4 2 9 . 5 2 1 2 9 . 6 1 3 2 9 . 6 4 5 2 9 . 6 8 3 2 9 . 7 3 4 2 9 . 7 8 2 3 1 . 9 9 2 3 2 . 0 1 0 3 2 . 5 3 7 3 2 . 6 7 4 3 3 . 0 8 2 3 3 . 6 3 1 3 4 . 6 1 6 4 8 . 8 1 0 4 8 . 9 8 2 4 9 . 1 5 3 4 9 . 3 2 3 4 9 . 4 9 5 4 9 . 6 6 5 4 9 . 8 3 6 5 1 . 3 1 5 7 0 . 2 1 2 7 2 . 1 5 8 7 4 . 4 6 2 7 6 . 9 7 0 7 7 . 2 2 5 7 7 . 4 8 0 8 5 . 1 7 3 8 5 . 2 8 3 1 2 9 . 6 3 4 1 3 1 . 1 7 9 1 7 5 . 8 1 6 PC 1.00 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7577678 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 22.00 dB PL12 14.68 dB PL2 −3.00 dB PCPD2 88.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7703643 MHz PL1 −1.00 dB P1 10.50 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 303.5 K DE 6.00 usec DW 16.650 usec RG 8192 AQ 1.0912410 sec FIDRES 0.458222 Hz SWH 30030.029 Hz DS 2 NS 3072 SOLVENT CDCl3 TD 65536 PULPROG zgpg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 20.45 Date_ 20090601 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111THU_WEDE.FC4 Current Data Parameters 1' 8 9 4 3 2' 1 2 19 27'18 26' 4' 6 17 25' 3' WEDE.FC4−CDCl3&MeOD−C13CPD 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm DEPT90 DEPT135 C13CPD CH&CH3 CH2 &DEPT Phuï luïc 44: Phoå D E PT cuûa hôïp chaát W E D E .FC 4 1' 8 9 4 3 2' 1 2 3' 17 25' 6 4' 18 26' 19 27' ppm 1.01.52.02.53.03.54.04.55.05.5 ppm 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 WEDE.FC4−CDCl3&MeOD−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1299774 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1299798 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −3.00 dB P1 10.50 usec P0 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 303.5 K DE 6.00 usec DW 100.000 usec RG 287.4 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm Multinucl INSTRUM av500 Time 21.40 Date_ 20090601 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111THU_WEDE.FC4 Current Data Parameters Phuï luïc 45: Phoå C O SY cuûa hôïp chaát W E D E .FC 4 8 9 2 1 2' 3 4 1 7 10 3' 5 3' 6 4' 19 27' 89 2 1 2' 3 4 1 7 3' 53' 64' 1927' p p m 1 . 01 . 52 . 02 . 53 . 03 . 54 . 04 . 55 . 05 . 5 p p m 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 W E D E . F C 4 − C D C l 3 & M e O D − H S Q C 8 9 2 1 2 ' 3 4 1 7 1 0 3 ' 5 3 ' 6 4 1 9 2 7 ' ' 1 9 2 7 ' 1 8 2 6 ' 4 ' 6 1 7 2 5 ' 3 ' 2 1 2 ' 3 4 8 9 p p m 0 . 81 . 01 . 21 . 41 . 61 . 82 . 02 . 2 p p m 1 3 1 4 1 5 1 6 1 7 1 8 1 9 2 0 2 1 2 2 2 3 2 4 2 5 2 6 2 7 2 8 2 9 3 0 3 1 3 2 3 3 3 4 3 5 3 6 W E D E . F C 4 − C D C l 3 & M e O D − H S Q C 1 9 2 7 ' 1 8 2 6 ' 4 ' 6 1 7 2 5 ' 7 1 0 5 3 ' 7 1 0 3 ' 3 ' 5 6 4 ' 1 9 2 7 ' P h u ï l u ï c 4 6 a : P h o å H S Q C c u û a h ô ï p c h a á t W E D E . F C 4 p p m 1 . 01 . 52 . 02 . 53 . 03 . 54 . 04 . 55 . 05 . 5 p p m 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 W E D E . F C 4 − C D C l 3 & M e O D − H M B C 8 9 2 1 2 ' 3 4 1 7 1 0 3 ' 5 3 ' 6 4 ' 1 9 2 7 ' 1 9 2 7 ' 1 8 2 6 ' 4 ' 6 1 7 2 5 ' 3 ' 2 1 2 ' 3 4 8 9 1 ' p p m 0 . 81 . 01 . 21 . 41 . 61 . 82 . 02 . 2 p p m 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 3 2 3 4 3 6 W E D E . F C 4 − C D C l 3 & M e O D − H M B C 7 1 0 3 ' 5 3 ' 6 4 ' 1 9 2 7 ' 1 9 2 7 ' 1 8 2 6 ' 4 ' 6 7 1 0 5 3 ' 1 7 2 5 ' P h u ï l u ï c 4 7 a : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F C 4 WEDE.FC6−CDCl3−1H 9 8 7 6 5 4 3 2 1 0 ppm − 0 . 0 0 6 0 . 0 0 0 0 . 0 0 6 1 . 5 5 9 2 . 1 4 2 2 . 1 5 6 2 . 1 6 6 2 . 1 7 7 2 . 1 9 0 2 . 4 9 8 2 . 5 1 4 2 . 5 2 6 2 . 5 4 2 2 . 5 6 2 2 . 5 7 5 2 . 5 8 9 2 . 6 0 2 3 . 5 0 9 3 . 5 2 0 3 . 5 2 6 3 . 5 3 8 3 . 8 2 5 3 . 8 9 8 3 . 9 1 1 3 . 9 1 5 3 . 9 2 8 5 . 4 6 4 6 . 5 0 5 6 . 5 0 9 6 . 5 7 4 6 . 5 7 7 6 . 5 9 0 6 . 5 9 3 6 . 7 8 9 6 . 8 0 5 7 . 2 5 8 1 . 1 2 1 2 . 2 1 2 1 . 0 9 3 1 . 0 9 4 0 . 9 8 3 1 . 0 2 7 1 . 0 4 4 1 . 0 0 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300000 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −3.00 dB P1 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 305.4 K DE 6.00 usec DW 50.000 usec RG 362 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 17.34 Date_ 20090722 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FC6 Current Data Parameters 5 6 2 OH 9 9 7 8 W E D E . F C 6− CD Cl 3− 1H 5. 5 5. 6 5. 7 5. 8 5. 9 6. 0 6. 1 6. 2 6. 3 6. 4 6. 5 6. 6 6. 7 6. 8 p p m 5.464 6.505 6.509 6.574 6.577 6.590 6.593 6.789 6.805 0.983 1.027 1.044 1.000 3. 6 3. 7 3. 8 3. 9 p p m 3.509 3.520 3.526 3.538 3.825 3.898 3.911 3.915 3.928 1.093 1.094 2. 2 2. 4 2. 6 p p m 2.142 2.156 2.166 2.177 2.190 2.498 2.514 2.526 2.542 2.562 2.575 2.589 2.602 1.121 2.212 5 6 2 O H 9 9 7 8 WEDE.FC6−CDCl3−C13CPD 200 180 160 140 120 100 80 60 40 20 ppm 0 . 0 0 0 3 9 . 2 5 5 4 6 . 5 0 9 5 5 . 8 2 3 7 3 . 3 0 6 7 6 . 7 6 9 7 7 . 0 2 2 7 7 . 2 7 6 1 1 1 . 1 4 8 1 1 4 . 1 6 3 1 2 1 . 3 6 7 1 3 2 . 3 4 6 1 4 3 . 9 8 4 1 4 6 . 4 6 4 PC 1.40 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7577856 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 22.00 dB PL12 14.68 dB PL2 −3.00 dB PCPD2 88.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7716224 MHz PL1 −1.00 dB P1 10.50 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 305.8 K DE 6.00 usec DW 15.900 usec RG 8192 AQ 1.0420883 sec FIDRES 0.479836 Hz SWH 31446.541 Hz DS 2 NS 3072 SOLVENT CDCl3 TD 65536 PULPROG zgpg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 18.42 Date_ 20090723 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111WEDE.FC6 Current Data Parameters 3 4 1 6 5 2 9 8 7 WEDE.FC6−CDCl3−C13CPD 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm 2030405060708090100110120130140150160170 ppm DEPT90 DEPT135 C13CPD CH&CH3 CH2 &DEPT Phuï luïc 51: Phoå D E PT cuûa hôïp chaát W E D E .FC 6 3 4 1 6 5 2 9 8 7 ppm 1.52.02.53.03.54.04.55.05.56.06.57.07.5 ppm 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 WEDE.FC6−CDCl3−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300151 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300154 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −3.00 dB P1 10.50 usec P0 10.50 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 314.8 K DE 6.00 usec DW 100.000 usec RG 1024 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm Multinucl INSTRUM av500 Time 19.48 Date_ 20090722 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111WEDE.FC6 Current Data Parameters Phuï luïc 52: Phoå C O SY cuûa hôïp chaát W E D E .FC 6 5 6 2 O H 9 9 7 8 5 6 2 O H 9 9 7 8 p p m 1234567 p p m 3 5 4 0 4 5 5 0 5 5 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 1 0 0 1 0 5 1 1 0 1 1 5 1 2 0 1 2 5 1 3 0 1 3 5 W E D E . F C 6 − C D C l 3 − H S Q C P h u ï l u ï c 5 3 : P h o å H S Q C c u û a h ô ï p c h a á t W E D E . F C 6 5 6 2 O H 9 9 7 8 7 8 9 2 5 6 1 p p m 234567 p p m 3 5 4 0 4 5 5 0 5 5 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 1 0 0 1 0 5 1 1 0 1 1 5 1 2 0 1 2 5 1 3 0 1 3 5 1 4 0 1 4 5 1 5 0 1 5 5 W E D E . F C 6 − C D C l 3 − H M B C P h u ï l u ï c 5 4 : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F C 6 5 6 2 O H 9 9 7 8 7 8 9 2 5 6 1 4 3 WEDE.FACE1−DMSO−1H 7 6 5 4 3 2 1 0 ppm 1 . 8 8 3 1 . 9 1 2 1 . 9 1 7 1 . 9 2 8 1 . 9 5 2 1 . 9 8 5 2 . 0 0 3 2 . 0 1 7 2 . 0 6 6 2 . 0 8 5 2 . 1 0 7 2 . 1 3 1 2 . 3 3 0 2 . 3 3 6 2 . 3 5 6 2 . 3 6 2 2 . 4 2 8 2 . 4 3 6 2 . 4 7 9 2 . 4 8 2 2 . 4 8 6 2 . 5 2 8 2 . 5 3 1 2 . 8 5 7 2 . 8 6 6 2 . 8 7 4 2 . 8 8 3 2 . 8 9 0 2 . 9 0 0 2 . 9 7 4 2 . 9 8 4 2 . 9 9 2 3 . 0 0 3 3 . 0 1 0 3 . 0 2 0 3 . 0 3 7 3 . 0 4 0 3 . 0 4 8 3 . 0 5 2 3 . 0 6 7 3 . 0 7 1 3 . 0 8 4 3 . 0 9 4 3 . 1 0 2 3 . 1 1 1 3 . 1 1 9 3 . 1 2 9 3 . 1 4 6 3 . 1 5 7 3 . 1 8 0 3 . 1 8 6 3 . 2 0 7 3 . 2 2 4 3 . 2 4 7 3 . 2 6 0 3 . 2 8 5 3 . 2 5 6 5 . 1 7 4 4 . 7 5 4 3 . 6 7 8 4 . 1 3 7 4 . 8 5 8 4 . 1 2 6 2 . 3 5 8 3 . 9 3 7 5 . 4 3 5 1 . 1 0 5 2 . 9 0 6 2 . 0 9 9 0 . 5 4 5 0 . 9 3 8 1 . 0 7 3 1 . 0 3 0 1 . 1 6 2 1 . 1 3 7 1 . 2 2 5 2 . 1 0 3 1 . 2 7 4 1 . 1 0 1 1 . 0 3 6 1 . 0 1 5 2 . 1 1 7 0 . 9 9 2 0 . 5 7 3 0 . 5 5 6 1 . 0 0 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300141 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −3.00 dB P1 5.85 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 301.4 K DE 6.00 usec DW 50.000 usec RG 64 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT DMSO TD 65536 PULPROG zg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 10.51 Date_ 20081020 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FACE1 Current Data Parameters 6a 6b 22a 23a 5a 5b 6a 6b 1' a 1' b 22 a 23 a

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