HRID1589

反应详情

EQUATION

反应方程式

HRID 1589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1-isoquinolinecarboxylic acid (50 g, 0.288 mol) in EtOH (150 mL) and 60 mL of 5N HCl was reduced over 5% Rh/Al2O3 (14 g) at 52 bar (750 psi) of hydrogen in a high pressure apparatus at 50° C. for 17 hours. The reaction mixture was filtered through a pad of diatomaceous earth, and the filtrate was concentrated in vacuo. The solid was triturated with water, filtered and dried to give DL-perhydro-1-isoquinolinecarboxylic acid (DL-1-Piq-OH) (30 g, 48%) FD-MS 184 (MH+).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a pad of diatomaceous earth
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe solid was triturated with water
  4. filtrationfiltered
  5. customdried