HRID1682447

反应详情

EQUATION

反应方程式

HRID 1682447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.5 g of 4-cyanobenzenesulfonyl chloride in 20 ml of dichloromethane was added dropwise with ice-cooling to a solution of 2.37 g of 7-(n-butyl)-9,9-dimethyl-3,7-diazabicyclo[3.3.1]nonane in 30 ml of dichloromethane. The ice-cooling was then removed, and the reaction mixture was stirred at room temperature for one hour. The hydrochloride of the title compound was thereupon deposited as a white precipitate. The crystals were filtered out with suction and dried at 60° C. in a vacuum drying oven. 2.5 g of 7-(n-butyl)-3-[(4-cyanophenyl)sulfonyl]-9,9-dimethyl-3,7-diazabicyclo[3.3.1]nonane hydrochloride having a melting point of 98° to 99° C. were obtained.

WORKUP

后处理

  1. customwas then removed
  2. filtrationThe crystals were filtered out with suction
  3. customdried at 60° C. in a vacuum
  4. customdrying oven