반응식
[CH:1]1[CH:2]=[CH:3][N:4]2[CH2:10][C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[N:7]([C:15]([C:17]3[CH:25]=[CH:24][C:20]([C:21]([OH:23])=O)=[CH:19][CH:18]=3)=[O:16])[CH2:6][C:5]=12.C(N(CC)CC)C.Cl.[CH3:34][C:35]1[C:41]([CH3:42])=[CH:40][CH:39]=[CH:38][C:36]=1[NH2:37].C(P(C#N)(CC)=O)C>ClCCl>[CH3:34][C:35]1[C:41]([CH3:42])=[CH:40][CH:39]=[CH:38][C:36]=1[NH:37][C:21](=[O:23])[C:20]1[CH:19]=[CH:18][C:17]([C:15]([N:7]2[C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=3[CH2:10][N:4]3[CH:3]=[CH:2][CH:1]=[C:5]3[CH2:6]2)=[O:16])=[CH:25][CH:24]=1참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
A mixture of 0.332 g of 4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)benzoic acid, 0.222 g of triethylamine, 0.157 g of 2,3-dimethylaniline hydrochloride, 0.15 ml of diethylphosphoryl cyanide in 20 ml of dichloromethane is heated on a steam bath for 3 hours. The mixture is washed with H2O, 1M NaHCO3, H2O, 1N HCl, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filter cake washed with dichloromethane. The filtrate is concentrated to dryness under vacuum and the residue crystallized from dichloromethane-hexane to give 0.11 g of crystals, m.p. 239°-240° C.
후처리
- temperatureis heated on a steam bath for 3 hours
- washThe mixture is washed with H2O, 1M NaHCO3, H2O, 1N HCl, brine
- dry with materialdried (Na2SO4)
- filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
- washthe filter cake washed with dichloromethane
- concentrationThe filtrate is concentrated to dryness under vacuum
- customthe residue crystallized from dichloromethane-hexane
출처 및 근거
- ORD 기록
- ord-0a78373a1e08482eb0f5451feb45d468
- 출처 데이터셋
- uspto-grants-1996_05
- 특허 번호
- US05516774
연결된 노트
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