HRID35234

反应详情

EQUATION

反应方程式

HRID 35234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-(4-Nitrophenethyl)-1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline hydrochloride (14.1 g, 0.037 m) was dissolved in methanol (500 ml) containing 10 ml of conc HCl and hydrogenated in a Parr apparatus over 5% Pd/C catalyst (1.5 g) at 40 psi for 1 hour. The catalyst was removed by filtration and the solvent volume reduced to ca 150 ml at an aspirator. Ethanol (100 ml) and ether (50 ml) were added and the mixture was hot filtered and allowed to stand overnight. The crystallized solid was collected by filtration and vacuum dried to give 12.8 g of N-(4-aminophenethyl)-1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline dihydrochloride, m.p. 259°-261°.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. additionEthanol (100 ml) and ether (50 ml) were added
  3. filtrationthe mixture was hot filtered
  4. filtrationThe crystallized solid was collected by filtration and vacuum
  5. customdried