Flumazenil → isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo [1,5-a][1,4]benzodiazepine-3-carboxylate

HRID 67343

反応式

HRID 67343 の反応式
[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][N:10]([CH3:22])[C:9](=[O:23])[C:8]=2[CH:24]=1.[CH3:25]C(O)C>>[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][CH:20]([CH3:25])[CH3:21])=[O:18])=[C:12]3[CH2:11][N:10]([CH3:22])[C:9](=[O:23])[C:8]=2[CH:24]=1

参加物

4

反応物 3

HCID 3373FlumazenilHCID 3776IsopropanolHCID 24758Sodium hydride

生成物 1

HCID 20515336isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo [1,5-a][1,4]benzodiazepine-3-carboxylate

実験手順

100 ml of 2-propanol are treated with 100 mg of sodium hydride. 5 g of ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate are added thereto and the mixture is heated to boiling under reflux for 1 hour. Subsequently, the mixture is left to cool to room temperature, the separated crystals are filtered off and washed with 2-propanol and water, there being obtained isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 243°-244° C.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 1 hour
  3. waitSubsequently, the mixture is left
  4. filtrationthe separated crystals are filtered off
  5. washwashed with 2-propanol and water, there

出典と根拠

ORDレコード
ord-aeea20da711e4ac3bab8ae3896857411
出典データセット
uspto-grants-1982_08
特許番号
US04346031

関連ノート

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