反应详情

温度

50 °C

A mixture of 12.85 g (0.05 moles) of 1-(3,4-dimethoxyphenyl)-2-nitro-1,3-propanediol, 20.4 g of acetic anhydride and 3.92 g of acetyl chloride is stirred at 50° C. for 5 hours. The mixture is cooled and poured onto ice. The resulting oily substance is washed twice with ice-cold water and decanted. Crystallization sets in after adding 20 ml of isopropanol to the substance. The separated crystalline product is filtered off, washed thrice with 5 ml of isopropanol and 10 ml of n-hexane, each, and dried. 11.1 g (65.1%) of the title compound are obtained; m.p.: 85°-88° C.

1. temperatureThe mixture is cooled
2. additionpoured onto ice
3. washThe resulting oily substance is washed twice with ice-cold water
4. customdecanted
5. customCrystallization sets
6. additionin after adding 20 ml of isopropanol to the substance
7. filtrationThe separated crystalline product is filtered off
8. washwashed thrice with 5 ml of isopropanol and 10 ml of n-hexane
9. customeach, and dried