Acetic Anhydride → HCID 11428649、化合物
反応式
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[CH2:6][C:7]([CH3:21])=[N:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[C:13]([CH3:20])[CH:12]=3)[C:4]=2[CH:3]=1.[C:24](OC(=O)C)(=[O:26])[CH3:25]>>[C:24]([N:8]1[C:7]([CH3:21])=[CH:6][C:5]2[CH:22]=[CH:23][C:2]([Cl:1])=[CH:3][C:4]=2[C:10]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[C:13]([CH3:20])[CH:12]=2)=[N:9]1)(=[O:26])[CH3:25]参加物
3
実験手順
A solution of 1.5 g (4.6 mmoles) of 8-chloro-4-methyl-1-(3-methyl-4-nitrophenyl)-5H-2,3-benzodiazepine in 15 ml of acetic anhydride is stirred in an oil bath of 130 to 140° C. for 5 hours. The reaction mixture is poured onto about 200 g of crushed ice and the separated crystals are filtered off. The crude product is recrystallized from acetonitrile. Thus 0.78 g (46%) of the desired compound melting at a temperature of 192 to 194° C. is obtained.
後処理
- filtrationthe separated crystals are filtered off
- customThe crude product is recrystallized from acetonitrile
- custommelting at a temperature of 192 to 194° C.
- customis obtained