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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethanol → (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid

HRID 223338
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인쇄 미리보기

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HRID 223338 반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18]CC)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].C(O)C>O>[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([OH:18])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 53890667ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]-benzodiazepine-1-carboxylate

생성물 1

HCID 22828765(S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

15 g (43.4 mmol) of ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate and 1.85 g (46.3 mmol) of sodium hydroxide are treated with 60 ml of ethanol and 10 ml of water, then heated to boiling under reflux for 45 minutes, the ethanol is subsequently distilled off in vacuo, the residue is treated with 46.5 ml of 1 N hydrochloric acid and left to stand in an ice-bath for 2 hours. The precipitated material is filtered off under suction, washed with water and dried to constant weight. There is obtained (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid which has a decomposition point of 265°.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 45 minutes
  3. distillationthe ethanol is subsequently distilled off in vacuo
  4. additionthe residue is treated with 46.5 ml of 1 N hydrochloric acid
  5. waitleft
  6. filtrationThe precipitated material is filtered off under suction
  7. washwashed with water
  8. customdried to constant weight

출처 및 근거

ORD 기록
ord-5e7b6bb01037448aae908d1a673e76e6
출처 데이터셋
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04353827

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