HRID365408

反应详情

EQUATION

反应方程式

HRID 365408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6.4 g of (+/-)-cis-1,2-dimethoxy-4-(2-aminocyclohexyl)benzene are dissolved in 150 ml of methylene chloride and 9 ml of triethylamine. A solution of 11.2 g of 4-p-toluenesulfonamidobenzoyl chloride in 200 ml of methylene chloride is added dropwise at RT in the course of 3 h, and the mixture is extracted after stirring for 1 h with 100 ml each of water, 2N hydrochloric acid, satd. sodium hydrogencarbonate solution and water again. The organic phase is dried using sodium sulfate, concentrated and crystallized from ethyl acetate. 3.9 g (28.2% of theory) of the title compound of m.p. 174-176° C. are obtained.

WORKUP

后处理

  1. extractionthe mixture is extracted
  2. customThe organic phase is dried
  3. concentrationconcentrated
  4. customcrystallized from ethyl acetate