7-chloro-4,5-dihydro-3-(hydroxymethyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one → 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde
反応式
[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[CH2:16][OH:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1>[O-2].[O-2].[Mn+4].C(Cl)Cl>[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[CH:16]=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
18.0 g (64.8 mmol) of 7-chloro-4,5-dihydro-3-hydroxymethyl-5methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one, 75 g of manganese dioxide and 700 ml of methylene chloride are stirred at room temperature for 1.5 hours. The reaction mixture is filtered and the filtrate is evaporated. By recrystallization of the residue from alcohol there is obtained 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde of melting point 204°-205°.
後処理
- filtrationThe reaction mixture is filtered
- customthe filtrate is evaporated
- customBy recrystallization of the residue from alcohol
出典と根拠
- ORDレコード
- ord-73709b47a02c461482d032f18ff8f961
- 出典データセット
- uspto-grants-1988_10
- 特許番号
- US04775671
反応ノート
読み込み中…