反应详情

19.6 g (0.1 moles) of 3,4,5-trimethoxybenzaldehyde and 9.1 g (0.1 moles) of nitroethanol are suspended in a mixture of 25 ml of methanol and 1 ml of N-methylpiperidine at a temperature of 0° C. (under cooling with ice water). The reaction mixture is stirred for 6 hours, then 50 ml of chloroform are added, the mixture is allowed to stand at 0° C. for 72 hours and then acidified with 1 ml of acetic acid. The separated crystalline substance is filtered off, washed with chloroform and ice-cold (0° C.) water and dried. 19.7 g 68.64%) of 1-(3,4,5-trimethoxyphenyl)-2-nitro-1,3-propanediol are obtained; m.p.: 155°-159° C.

1. waitto stand at 0° C. for 72 hours
2. filtrationThe separated crystalline substance is filtered off
3. washwashed with chloroform and ice-cold (0° C.) water
4. customdried