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 67298

反応式

HRID 67298 の反応式
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

参加物

3

反応物 1

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

生成物 1

HCID 6426758N-Desmethylflumazenil

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2cbbc12dcaef494d83ac5fc3ecd5235f
出典データセット
uspto-grants-1982_08
特許番号
US04346030

関連ノート

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