HRID67926

反应详情

EQUATION

反应方程式

HRID 67926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne (9.78 g) in anhydrous diethyl ether (12.5 ml) was treated with a solution of methanesulphonic acid (2.40 g) in anhydrous diethyl ether (12.5 ml), stirred and cooled. The solid precipitate was removed by filtration, washed with cold anhydrous diethyl ether and dried at 0.05 mm Hg for 2 hours, to give 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne methanesulphonate (11.61 g), m.p. 164°-165° C., in the form of a white powder which had the elementary analysis C: 51.3%; H: 5.49%; N: 2.60% (C21H27F6NO3S requires C: 51.73%; H: 5.58%; N: 2.87%).

WORKUP

后处理

  1. temperaturecooled
  2. customThe solid precipitate was removed by filtration
  3. washwashed with cold anhydrous diethyl ether
  4. customdried at 0.05 mm Hg for 2 hours