Acetic Anhydride → HCID 11013758、化合物
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][NH:9][CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1.[C:23](OC(=O)C)(=[O:25])[CH3:24]>>[C:23]([N:9]1[CH:8]([CH3:21])[CH2:7][C:6]2[CH:22]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[C:11]([C:12]2[CH:13]=[CH:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=2)=[N:10]1)(=[O:25])[CH3:24]参加物
3
実験手順
0.72 g (2.2 mmoles) of 7-chloro-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine are stirred in 4 ml of acetic anhydride at 25° C. for 3 hours, then the reaction mixture is poured onto 20 ml of ice water, the crystalline product is filtered and washed with water several times. The crude product obtained is purified by suspending it in 4 ml of hot ethanol. After filtration and drying, 0.69 g (88%) of the title compound are obtained M.p.: 174°-175° C.
後処理
- filtrationthe crystalline product is filtered
- washwashed with water several times
- customThe crude product obtained
- customis purified
- filtrationAfter filtration