反应详情

温度

25 °C

0.8 ml (13.4mmol) of methyl isocyanate was added to a solution containing 1.0 g (3.41 mmol) of 1-(4-aminophenyl)-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine in 8 ml of dimethylformamide (DMF), then the reaction mixture was stirred at 25° C. for 24 hours. After diluting with 80 ml of water, filtering at 5° C. and drying at 60° to 100° C., 1.06 g of raw product, m.p.: 204°-207° C. (sintering from 160° C.) were obtained which, when recrystallized from 5 ml of ethanol, gave 0.85 g (71.4%) of the aimed product, m.p.: 223°-224° C. (decomp.).

1. filtrationfiltering at 5° C.
2. customdrying at 60° to 100° C.
3. custom1.06 g of raw product, m.p.: 204°-207° C. (sintering from 160° C.) were obtained which, when
4. customrecrystallized from 5 ml of ethanol