Flumazenil → Flumazenil Impurity 8

HRID 67489

反応式

HRID 67489 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]([O:17][CH2:18]C)=[O:16])=[C:10]3[CH2:9][N:8]([CH3:20])[C:7](=[O:21])[C:6]=2[CH:22]=1.[C-]#N.[K+]>CO>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]([O:17][CH3:18])=[O:16])=[C:10]3[CH2:9][N:8]([CH3:20])[C:7](=[O:21])[C:6]=2[CH:22]=1

参加物

4

反応物 2

HCID 3373FlumazenilHCID 9032Potassium Cyanide

生成物 1

HCID 20515347Flumazenil Impurity 8

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 3.5 g (11.5 mmol) of ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 0.15 g of potassium cyanide and 40 ml of methanol is stirred at the boiling point for 2.5 hours. The solvent is distilled off on a rotary evaporator and the residue is taken up in chloroform. After filtration from insoluble material, the filtrate is concentrated. After recrystallisation of the residue from ethyl acetate, there is obtained methyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 195°-196.5° C.

後処理

  1. distillationThe solvent is distilled off on a rotary evaporator
  2. filtrationAfter filtration from insoluble material
  3. concentrationthe filtrate is concentrated
  4. customAfter recrystallisation of the residue from ethyl acetate

出典と根拠

ORDレコード
ord-7707367bc4b04173954be4eef17bcc3c
出典データセット
uspto-grants-1982_08
特許番号
US04346033

関連ノート

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