三乙胺 → 10-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepine

HRID 3582

反应方程式

HRID 3582 反应方程式
[NH2:1][C:2]1[CH:23]=[CH:22][C:5]([C:6]([N:8]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[CH2:12][N:11]3[CH:19]=[CH:20][CH:21]=[C:10]3[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:31]1([P:37](Cl)([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)=[O:38])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[OH-].[Na+]>ClCCl>[C:31]1([P:37]([NH:1][C:2]2[CH:23]=[CH:22][C:5]([C:6]([N:8]3[C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=4[CH2:12][N:11]4[CH:19]=[CH:20][CH:21]=[C:10]4[CH2:9]3)=[O:7])=[CH:4][CH:3]=2)([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)=[O:38])[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1

参与物

6

反应物 4

HCID 8471三乙胺HCID 14798二甲基对苯二胺二盐酸HCID 73910二苯基次膦酰氯HCID 1082828010,11-dihydro-10(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

产物 1

HCID 1534067810-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepine收率 96.4%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

A mixture of 0.10 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine 0.060 g of triethylamine and 0.12 g of diphenylphosphinyl chloride in 2 ml of dichloromethane is stirred at room temperature for 2 hours and then 1N NaOH is added. The mixture is extracted with ethyl acetate and the extract washed with brine and dried (Na2SO4). The solvent is removed and the residue triturated with ether-hexane to give 0.16 g of a white solid.

后处理

  1. extractionThe mixture is extracted with ethyl acetate
  2. washthe extract washed with brine
  3. dry with materialdried (Na2SO4)
  4. customThe solvent is removed
  5. customthe residue triturated with ether-hexane

来源与证据

ORD记录
ord-de0f1607b1fa4c449eebf6846c063d59
来源数据集
uspto-grants-1998_03
专利号
US05733905

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