菲并吲哚里西啶生物碱季铵盐衍生物及其制备和抗植物病毒应用_2

文档序号:9410185阅读:来源:国知局
,3. 65 (br, 2H),2. 50-2. 40(m,1H),2. 31-2. 22(m,2H),2. 00(s,3H),1. 94-1. 80(m,1H);13CNMR(100MHz, DMS0-d6)S149. 9,149. 5,149. 5,149. 4,124. 6,124. 1,124. 0,123. 7,123. 1,118. 8,105. 0, 104.1,104. 1,88. 6,68. 7,67. 3,63. 2,56. 5,56. 5,56. 4,56. 1,55. 4,53. 6,51. 6,28. 9,25.1, 20. 1,3. 9 ;HRMS(ESI)calcdforC28H32N04+[M-Br]446. 2326,found446. 2331.
[0037]化合物I-R-2a:白色固体,Mp:222_223°C?Yield:22 % 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-2a相同.
[0038]化合物I-S_2b
[0039] 白色固体.Mp:240-242°C.Yield:24%. 4NMR(400MHz,DMS0-d6)S8. 16(s,lH), 8. 14(s,1H),7. 43(s,1H),7. 34(s,1H),5. 57(d,J= 16. 0Hz,1H),4. 99(d,J= 16. 0Hz,1H), 4. 38-4. 35 (m,4H),4. 12 (s,6H),4. 04 (s,3H),4. 03 (s,3H),3. 88-3. 60 (m,2H),3. 40-3. 26 (m, 1H),2. 50(br,1H),2. 34-2. 24(m,2H),2. 20-2. 10(m,1H),1. 98(s,3H);13C匪R(100MHz, DMS0-d6)S149. 4,149. 1,149. 0,148. 8,123. 8,123. 8,123. 7,123. 6,122. 5,118. 5,104. 5, 104. 0,103. 3,88. 7,68. 6,67. 5,61. 4,58. 5,56. 0,56. 0,55. 6,55. 0,42. 2,26. 2,25. 3,18. 6, 3. 4 ;HRMS(ESI)calcdforC27H30N04+[M-Br]432. 2169,found432.2177.
[0040]化合物I-R-2b:白色固体,Mp:240-243°C?Yield:30 % 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-2b相同.
[0041]化合物I-S_3a
[0042]浅黄色固体.Mp:212-215°C?Yield:45% ? 4NMR(400MHz,DMS0-d6)S8.ll(s, 1H),8. 10(s,1H),7. 49(s,1H),7. 44(s,1H),5. 32(d,J= 16. 0Hz,1H),5. 15(d,J= 16. 0Hz, 1H),5. 07(s,2H),4. 40-4. 38(m,1H),4. 07(s,6H),4. 02(s,3H),4. 00(s,3H),3. 74-3. 63(m, 2H),2. 48-2. 45(m,1H),2. 31-2. 27(m,2H),1. 94-1. 84(m,1H).13CNMR(100MHz,DMS0-d6) S149. 6,149. 1,149. 0,149. 0,124. 4,123. 7,123. 5,123. 4,122. 5,117. 8,112. 5,104. 5, 104. 3,103. 6,69. 7,65. 0,56. 0,55. 9,55. 6,55. 0,48. 7,28. 6,25. 3,20. 1.HRMS(ESI)calcd forC26H29N204+[M-Br]433. 2122,found433. 2127.
[0043]化合物I-R-3a:浅黄色固体,Mp:212_214°C.Yield:44% ? 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-3a相同.
[0044]化合物I-S_3b
[0045]浅黄色固体,Mp:217-219°C?Yield:28% ? 4NMR(400MHz,DMS0-d6)S8. 10(s, 1H),8. 06(s,1H),7. 37 (s,1H),7. 31 (s,1H),5. 54(d,J= 16. 0Hz,1H),5. 21 (d,J= 16.0Hz,lH),4.98(d,J=16.8Hz,lH),4.81(d,J= 16.8Hz,lH),4.44-4.36(m,lH), 4. 29-4. 22(m,1H),4. 06(s,3H),4. 05(s,3H),4. 00(s,3H),3. 98(s,3H),4. 01-3. 95(m,1H), 3. 88-3. 83 (m,1H),3. 24-3. 19 (m,1H),2. 58-2. 55 (m,1H),2. 43-2. 31 (m,2H),2. 23-2. 13 (m, 1H).13CNMR(100MHz,DMS0-d6)S149.5,149.2,149.0,148.9,124.0,123.9,123.7,123.3, 122. 4,118. 1,112. 5,104. 5,104. 1,103. 4, 70. 5, 64. 1,60. 8, 56. 0,55. 6, 41. 1,26. 2, 25. 1, 18. 8.HRMS(ESI)calcdforC26H29N204+[M-Br]433. 2122,found433. 2127.
[0046]化合物I-R-3b:浅黄色固体Mp:216-220°C.Yield:30% ? 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-3b相同.
[0047]化合物I-S_4a
[0048]白色固体,Mp:173-175°C?Yield:47 % 4NMR(400MHz,DMS0-d6)S8. 10(s, 1H),8. 09(s,1H),7. 47(s,1H),7. 34(s,1H),5. 28(d,J= 16. 0Hz,1H),5. 07(d,J=16. 0Hz, 1H),4. 57-4. 43(m,3H),4. 19(q,J= 6. 8Hz,2H),4. 06(s,3H),4. 06(s,3H),3. 99(s,3H), 3. 98 (s,3H),3. 99-3. 98 (m,2H),3. 74-3. 68 (m,1H),2. 43-2. 38 (m,1H),2. 27-2. 14 (m,2H), 1. 80-1. 68 (m,1H),1. 19 (t,J= 6. 8Hz,3H) ?13C匪R(100MHz,DMS0-d6)S165. 3,149. 5, 149. 1,149. 0,124. 2,123. 7,123. 6,123. 5,122. 7,118. 3,104. 5,104. 2,103. 4,69. 8,64. 0, 62. 0,59. 4,56. 0,55. 8,55. 6,53. 4,28. 2,25. 3,20. 0,13. 7.HRMS(ESI)calcdforC2SH34N06+[ M-Br]480. 2381,found480. 2384.
[0049]化合物I-R-4a:白色固体,Mp:175_176°C?Yield:42 % 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-4a相同.
[0050]化合物I-S_4b
[0051]白色固体?Mp:174-177°C?Yield:40 % 4NMR(400MHz,DMS0-d6)S7. 86(s, 1H),7. 84(s,1H),7. 13(s,1H),6. 95(s,1H),5. 52(d,J= 17. 2Hz,1H),4. 86(d,J= 16. 0Hz, 1H),4. 30-4. 27(m,1H),4. 05-3. 99(m,2H),3. 90(q,J=7. 2Hz,2H),3. 90-3. 78(m,7H), 3. 75-3. 73(m,7H),3. 66-3. 44(m,2H),2. 28(br,1H),2. 13-1. 91(m,3H),0? 86(t,J=7. 2Hz, 3H).13CNMR(100MHz,DMS0-d6)S165. 1,149. 4,149. 1,148. 9,148. 8,123. 9,123. 7,123. 4, 122. 5,118. 6,104. 5,104. 1,103. 1,71. 8, 62. 5,62. 1,59. 4, 56. 0,55. 9,55. 6,48. 9,26. 2, 24.9,18. 8,13. 6.HRMS(ESI)calcdforC28H34N06+[M-Br]480. 2381,found480. 2387.
[0052]化合物I-R-4b:白色固体?Mp:169-171°C?Yield:46 % 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-4b相同.
[0053]化合物I-S_5a
[0054]浅黄色固体.Mp:211-215°C?Yield:40 % 4NMR(400MHz,DMS0-d6)S8.ll(s, 1H),8. 10 (s,1H),7. 83 (s,1H),7. 71 (s,1H),7. 46 (s,1H),7. 31 (s,1H),5. 38 (d,J= 16. 4Hz, 1H),4. 90(d,J= 16. 4Hz,1H),4. 30(br,1H),4. 17-4. 12(m,10H),3. 98(s,3H),3. 97(s, 6H),3. 68-3. 56 (m,2H),2. 45-2. 39 (m,1H),2. 28-2. 19 (m,2H),1. 88-1. 78 (m,1H) ?13C NMR(100MHz,DMS0-d6)S165. 6,149. 5,149. 1,149. 0,148. 9,124. 2,123. 7,123. 53,122. 8, 122. 6,118. 2,104. 5,104. 3,103. 4,68. 8,63. 6,59. 1,56. 0,55. 7,55. 6,53. 3,27. 7,25. 3, 19. 7.HRMS(ESI)calcdforC26H31N205+[M-Br]451. 2227,found451. 2236.
[0055]化合物I-R-5a:浅黄色固体,Mp:211-213°C.Yield:40% ? 4NMR,13CNMR,and HRMS(ESI)与化合物I-S-5a相同.
[0056]化合物I-S_5b
[0057]浅黄色固体.Mp:228-231°C.Yield:37. 5%.NMR(400MHz,DMS0-d6)S8. 10(s, 1H),8. 08 (s,1H),7. 87 (s,1H),7. 72 (s,1H),7. 41 (s,1H),7. 16 (s,1H),5. 96 (d,J= 16. 0Hz, 1H),4. 96(d,J= 16. 0Hz,1H),4. 57(br,1H),4. 23-4. 15(m,1H),4. 06(s,6H),3. 98(s,3H), 3. 95 (s,3H),3. 98-3. 95 (m,1H),3. 81-3. 69 (m,3H),3. 24-3. 16 (m,1H),2. 57-2. 53 (m,1H), 2. 35-2. 28(m,2H) ,2. 14-2. 03(m, 1H).13CNMR(100MHz,DMS〇-d6) 8 165.6,149.4,149.1, 148. 9,148. 9,123. 9,123. 9,123. 8,123. 4,122. 5,118. 8,104. 5,104. 4,104. 1,103. 0,71. 1, 62. 2,59. 1,56. 0,55. 8,55. 6,48. 6,26. 6,25. 3,18. 8.HRMS(ESI)calcdforC26H31N205+[M~ Br]451. 2227,found451. 2231.
[0058] 化合物I-R-5b:Paleyellowsolid,Mp:230-232°C.Yield:39%. 4NMR,13CNMR, andHRMS(ESI)与化合物I-S-5b相同.
[0059] 化合物I-S_6a
[0060] 黄色固体.Mp205-209°C?yield:35% ? 4NMR(400MHz,DMS0-d6)S8. 48(d,J =4. 4Hz,lH),8.10 (s,lH),8.09 (s,lH
当前第2页1 2 3 4 5 
网友询问留言 已有0条留言
  • 还没有人留言评论。精彩留言会获得点赞!
1