HRID46476

反应详情

EQUATION

反应方程式

HRID 46476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.9 g (0.0139 mole) of the free base, 3-(4-chlorophenyl)-N,N-dimethylindeno[1,2-c]pyrazole-2(4H)-propanamine, from Example 3C, in 25 ml of MeCN is treated with 1.35 g (0.0139 mole) of MeSO3H dissolved in 5 ml of MeCN. On seeding and rubbing, the crystalline mesylate salt separates; wt., after cooling overnight, 4.1 g (66%); m.p. 151°-153°. Following recrystallization from 20 ml of MeOH-100 ml ether, the cream-colored solid weighs 3.8 g (61%); m.p. 151°-153°.

WORKUP

后处理

  1. temperaturewt., after cooling overnight
  2. customrecrystallization from 20 ml of MeOH-100 ml ether