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Ammonia → Uxepam

HRID 66557
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HRID 66557 반응식
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:7]=2[CH:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:5]([C:20](Cl)=[O:21])[CH2:4][C:3]1=[O:23].[NH3:24]>CO>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:7]=2[CH:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:5]([C:20](=[O:21])[NH2:24])[CH2:4][C:3]1=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 20486168HCID 20486168, 화합물

생성물 1

HCID 68787Uxepam수율 72%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 1.7 g. (4.87 mmoles) of 1-methyl-4-chlorocarbonyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one in 3.5 ml. of concentrated ammonia and 7 ml. of methanol is stirred at room temperature overnight. The mixture is diluted with 30 ml. of water, the separated crude product is filtered off, and recrystallized from ethanol without drying. 1.16 g. (72%) of 1-methyl-4-carbamoyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one are obtained; m.p.: 212°-215° C.

후처리

  1. additionA suspension of 1.7 g
  2. additionThe mixture is diluted with 30 ml
  3. customof water, the separated crude product
  4. filtrationis filtered off
  5. customrecrystallized from ethanol
  6. customwithout drying

출처 및 근거

ORD 기록
ord-40bef482622245f78ab47a155d0a1cd7
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04342755

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