HRID479569

反应详情

EQUATION

反应方程式

HRID 479569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of acetic acid (0.72 kg, mol) in DME (13.6 L) was added dropwise to a stirred solution of (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidine (4.4 kg, 13.7 mol) in NMP (14 kg) at 100° C. After addition the thick slurry was allowed to cool and was stirred overnight at room temperature. The solid was collected by filtration, washed with DME (4.9 L) and dried overnight in vacuo at 50° C. to give (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidinium acetate (6 kg, 143%) as an NMP wet off white solid.

WORKUP

后处理

  1. additionAfter addition the thick slurry
  2. temperatureto cool
  3. filtrationThe solid was collected by filtration
  4. washwashed with DME (4.9 L)
  5. customdried overnight in vacuo at 50° C.