HRID1704235

反应详情

EQUATION

反应方程式

HRID 1704235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

100 kg. of 3,4-diethoxy-benzyl cyanide are hydrogenated in 310 1. of a 80 to 96% aqueous ethanol containing 9 to 12% of ammonia in the presence of 24 kg. of a Raney-nickel catalyst pretreated according to Example 3, at 45° to 68° C under a hydrogen overpressure of 8 to 10 atm. The catalyst is filtered off, the solution is evaporated and the residue is subjected to fractionation in vacuo. Thus 96 kg. of highly pure 3,4-diethoxy-beta-phenyl-ethylamine are obtained. The purity is almost 100%. The mono-desethylated beta-phenyl-ethylamine derivative is present at most in traces in such a small amount, which can not be detected by thin layer chromatography.

WORKUP

后处理

  1. custompretreated according to Example 3, at 45° to 68° C under a hydrogen overpressure of 8 to 10 atm
  2. filtrationThe catalyst is filtered off
  3. customthe solution is evaporated