HRID1493175

反应详情

EQUATION

反应方程式

HRID 1493175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (15.2 g) was added to a solution of 3-hydroxybenzaldehyde (48.8 g) and pyrrolidine (66.4 ml) in ethanol. After 18 hours the ethanol was removed and the residual oil was acidified with hydrochloric acid and washed with ethyl acetate. The aqueous solution was then basified with ammonia and extracted with ethyl acetate. Evaporation of the organic extracts yielded the title compound as an off-white solid (21.4 g), m.p. 100°-102°. TLC Silica; methanol; 0.88 ammonia (80:1)Rf 0.48.

WORKUP

后处理

  1. customAfter 18 hours the ethanol was removed
  2. washwashed with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. customEvaporation of the organic extracts