Hydrazine hydrate (1:1) → 3-Amino-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-one

HRID 258089

반응식

HRID 258089 반응식
[C:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[NH:11][C:10](=[O:18])[CH:9]([N:19]3C(=O)C4=CC=CC=C4C3=O)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.NN>O1CCCC1>[NH2:19][CH:9]1[N:8]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[NH:11][C:10]1=[O:18]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 14800302(3RS)-1,3-dihydro-5-phenyl-3-phthalimido-2H-1,4-benzodiazepine-2-one

생성물 1

HCID 42596493-Amino-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-one수율 67.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of (3RS)-1,3-dihydro-5-phenyl-3-phthalimido-2H-1,4-benzodiazepine-2-one (8.2 g), hydrazine hydrate (1.08 g) and tetrahydrofuran (160 ml) was stirred for 1.0 hour at room temperature and heated under reflux for 1.5 hours. After the precipitates were filtered off, the filtrate was evaporated to small volume and the equivalent volume of diisopropyl ether was added thereto. The precipitates were collected by filtration to give (3RS)-1,3-dihydro-3-amino-5-phenyl-2H-1,4-benzodiazepine-2-one (3.64 g).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 1.5 hours
  3. filtrationAfter the precipitates were filtered off
  4. customthe filtrate was evaporated to small volume
  5. additionthe equivalent volume of diisopropyl ether was added
  6. filtrationThe precipitates were collected by filtration

출처 및 근거

ORD 기록
ord-bd8e9bfe2d904515a7486e9d40512fef
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264433

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