反应详情

温度

60 °C

A mixture of 9.7 g (0.0337 moles) of 1-(3,4,5-trimethoxyphenyl)-2-nitro-1,3-propanediol, 13.78 g (0.135 moles) of acetic anhydride and 2.6 g of acetyl chloride is stirred at 60° C. for 4 hours. Thereafter the mixture is cooled to 20° C. and poured onto 50 g of ice. Crystallization sets in immediately. The separated product is filtered off, washed thrice with 15 ml of ice-cold water, each, and then with a small amount (about 3 ml) of isporopanol, and dried. 11.3 g (90.12%) of the title compound are obtained; m.p.: 107°-109° C.

1. temperatureThereafter the mixture is cooled to 20° C.
2. customCrystallization
3. filtrationThe separated product is filtered off
4. washwashed thrice with 15 ml of ice-cold water
5. customeach, and then with a small amount (about 3 ml) of isporopanol, and dried