HRID614287

反应详情

EQUATION

反应方程式

HRID 614287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of α-carbethoxy-α-diethoxymethyl-β-(3,4-dimethoxyphenyl)-propionitrile (3.75 g) 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 17 hours at reflux the mixture was allowed to cool and the product was filtered and washed with ethanol giving a white solid which was purified as described in Example 5 to yield 1.4 g (54%) of the title compound, m.p. 231°-233° C.

WORKUP

后处理

  1. temperatureat reflux for one hour
  2. temperaturereflux
  3. customreached 85° C
  4. temperatureAfter 17 hours at reflux the mixture
  5. temperatureto cool
  6. filtrationthe product was filtered
  7. washwashed with ethanol giving a white solid which
  8. customwas purified