HRID481471

反应详情

EQUATION

反应方程式

HRID 481471 的结构方程式

PROCEDURE

实验过程

A solution of 3.57 g (10 mmol) of 2-(1-chlorocyclopropyl)-1-(2-chlorophenyl)-3-(5-methylthio-1,2,4-triazol-1-yl)-propan-2-ol in 40 ml of glacial acetic acid is treated dropwise at 90° C. with stirring with 4 ml of an aqueous hydrogen peroxide solution (35% strength). After the addition has ended, stirring of the reaction mixture is continued at 90° C. for 30 minutes, and the mixture is then cooled to room temperature, treated with ice and rendered alkaline by adding aqueous sodium hydroxide solution. The mixture is extracted repeatedly using ethyl acetate, and the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. The slowly crystallizing product which remains is filtered off with suction. In this manner, 2.0 g (51% of theory) of 2-(1-chloro-cyclopropyl)-1-(2-chlorophenyl)-3-(5-methylsulphonyl-1,2,4-triazol-1-yl)-propan-2-ol) are obtained in the form of a solid which melts at 125°-128° C.

WORKUP

后处理

  1. additionAfter the addition
  2. additiontreated with ice
  3. extractionThe mixture is extracted repeatedly using ethyl acetate
  4. dry with materialthe combined organic phases are dried over sodium sulphate
  5. concentrationconcentrated under reduced pressure
  6. filtrationThe slowly crystallizing product which remains is filtered off with suction