反应详情

A solution of α-carbethoxy-α-diethoxymethyl-β-(4,5-dimethoxy-2-methylphenyl)propionitrile (3.9 g, 0.01 mol) and an equivalent amount of potassium hydroxide in ethanol (70 ml) was heated at reflux for one hour. A solution of guanidine (0.035 mol) in ethanol (50 ml) was added, and reflux was resumed. Ethanol was boiled off until the reaction temperature reached 85° C. After 20 hours at reflux the mixture was allowed to cool, and the product was filtered and washed with ethanol giving 2.57 g (94%) of nearly white solid. After purification as described in Example 5, the product was dried under reduced pressure giving a white solid, m.p. 231°-233° C.

1. temperatureat reflux for one hour
2. temperaturereflux
3. customreached 85° C
4. temperatureAfter 20 hours at reflux the mixture
5. temperatureto cool
6. filtrationthe product was filtered
7. washwashed with ethanol giving 2.57 g (94%) of nearly white solid
8. customAfter purification
9. customthe product was dried under reduced pressure
10. customgiving a white solid, m.p. 231°-233° C.