HRID1579315

反应详情

EQUATION

反应方程式

HRID 1579315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

30 G. of 4-cyano-3,5-dimethoxy-benzoic acid methyl ester and 1500 ml. of methanol and 150 ml. of 1N hydrochloric acid is hydrogenated in the presence of 10 g. of palladium-on carbon 10% at room temperature and under atmospheric pressure. In about 5 hours, 2 moles of hydrogen are taken up. The solution is freed of the catalyst by filtration, evaporated to dryness and the residue is taken up in a little water. The solution is thereafter filtered, saturated with solid potassium carbonate and shaken with benzene. From the shaken benzene mixture, is obtained 4-(aminomethyl)-3,5-dimethoxy-benzoic acid methyl ester, which after recrystallization from high boiling petroleum ether has a m.p. of 81°-83°.

WORKUP

后处理

  1. customat room temperature
  2. filtrationThe solution is freed of the catalyst by filtration
  3. customevaporated to dryness
  4. filtrationThe solution is thereafter filtered, saturated with solid potassium carbonate