ethyl 5-(2,4-dimethoxybenzyl)-8-fluoro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate → N-Desmethylflumazenil

HRID 67398

반응식

HRID 67398 반응식
COC1C=C(OC)C=CC=1C[N:6]1[C:12](=[O:13])[C:11]2[CH:14]=[C:15]([F:18])[CH:16]=[CH:17][C:10]=2[N:9]2[CH:19]=[N:20][C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:8]2[CH2:7]1>FC(F)(F)C(O)=O>[F:18][C:15]1[CH:16]=[CH:17][C:10]2[N:9]3[CH:19]=[N:20][C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:8]3[CH2:7][NH:6][C:12](=[O:13])[C:11]=2[CH:14]=1

참가 물질

3

반응물 1

HCID 20515335ethyl 5-(2,4-dimethoxybenzyl)-8-fluoro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate

생성물 1

HCID 6426758N-Desmethylflumazenil

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

13.0 g (29.6 mmol) of ethyl 5-(2,4-dimethoxybenzyl)-8-fluoro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate are heated to boiling under reflux for 4 hours in 45 ml of trifluoroacetic acid. After evaporation of the dark red suspension in vacuo, the residue is treated with water and made alkaline with ca 100 ml of 15 percent potassium carbonate solution. The separated material is filtered off under suction and washed with water. After recrystallisation from ca 500 ml of ethanol, there is obtained ethyl 8-fluoro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 298° C.

후처리

  1. customAfter evaporation of the dark red suspension in vacuo
  2. additionthe residue is treated with water
  3. filtrationThe separated material is filtered off under suction
  4. washwashed with water
  5. customAfter recrystallisation from ca 500 ml of ethanol

출처 및 근거

ORD 기록
ord-eabaf055b34f4c40b19493c52d9966f3
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346032

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