Water → Flumazenil

HRID 67350

반응식

HRID 67350 반응식
[H-].[Na+].[F:3][C:4]1[CH:5]=[CH:6][C:7]2[N:13]3[CH:14]=[N:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:12]3[CH2:11][NH:10][C:9](=[O:22])[C:8]=2[CH:23]=1.[CH3:24]I.O>CN(C)C=O>[F:3][C:4]1[CH:5]=[CH:6][C:7]2[N:13]3[CH:14]=[N:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:12]3[CH2:11][N:10]([CH3:24])[C:9](=[O:22])[C:8]=2[CH:23]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 6426758N-Desmethylflumazenil

생성물 1

HCID 3373Flumazenil

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.1 g (2 mmol) of sodium hydride (55 percent oil dispersion) are suspended in 10 ml of dry dimethylformamide and treated with 0.5 g (1.7 mmol) of ethyl 8-fluoro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate. After completion of the gas evolution, 0.13 ml (2 mmol) of methyl iodide is added and the mixture is stirred at room temperature for 2 hours. The mixture is poured into ca 60 ml of water and extracted three times with 30 ml of chloroform each time. The combined chloroform extracts are washed with ca 30 ml of water, dried over magnesium sulphate and evaporated. After recrystallisation from ethyl acetate, there is obtained ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 196°-197° C.

후처리

  1. extractionextracted three times with 30 ml of chloroform each time
  2. washThe combined chloroform extracts are washed with ca 30 ml of water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customAfter recrystallisation from ethyl acetate

출처 및 근거

ORD 기록
ord-974440ed808e4ce79112467fb0f8e4df
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346031

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