Water → t-butyl 8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

HRID 223340노트

반응식

HRID 223340 반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:26])[N:9]3[CH2:25][CH2:24][CH2:23][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16](N3C=CN=C3)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH2:27]>CN(C)C=O>[Cl:1][C:2]1[C:7]2[C:8](=[O:26])[N:9]3[CH2:25][CH2:24][CH2:23][CH:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:27][C:7]([CH3:8])([CH3:2])[CH3:6])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 54332091(S)-1-[(8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-1-yl)carbonyl]imidazole

생성물 1

HCID 20521886t-butyl 8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 1.1 g (3 mmol) of (S)-1-[(8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-1-yl)carbonyl]imidazole in 10 ml of dry dimethylformamide is treated while stirring with 0.34 g (3 mmol) of potassium t-butylate, the mixture is stirred at room temperature for a further 30 minutes, then poured into 200 ml of water and extracted three times with chloroform. The chloroform solution is washed three times with water, dried over magnesium sulphate and evaporated. After crystallization from ethyl acetate, there is obtained t-butyl 8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 223°-225°.

후처리

  1. additionis treated
  2. extractionextracted three times with chloroform
  3. washThe chloroform solution is washed three times with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customAfter crystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-0e44314d3ff7484492cc813c16e058ec
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04353827

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