反应详情

温度

25 °C

0.22 ml (2.04 mmol) of phenyl isocyanate was added to a solution of 0.50 g (1.7 mmol) of 1-(4-aminophenyl)-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine in 4 ml of dimethylformamide and the reaction mixture was stirred at 25° C. for one hour. Then it was diluted with 20 ml of diethyl ether and filtered at 5° C. The crystals were washed with 2×5 ml of diethyl ether and dried at 60°-100° C. The resulting 0.70 g of raw product, m.p. 239°-240° C. (sintering at 180° C.) was refluxed in 15 ml of ethanol, filtered after cooling, washed with 3×1 ml of ethanol and dried at 100° C. to yield 0.55 g (78.6%) of the aimed product, m.p. 240°-241° C. (decomp.).

1. filtrationfiltered at 5° C
2. washThe crystals were washed with 2×5 ml of diethyl ether
3. customdried at 60°-100° C
4. temperatureThe resulting 0.70 g of raw product, m.p. 239°-240° C. (sintering at 180° C.) was refluxed in 15 ml of ethanol
5. filtrationfiltered
6. temperatureafter cooling
7. washwashed with 3×1 ml of ethanol
8. customdried at 100° C.