HRID1389839

反应详情

EQUATION

反应方程式

HRID 1389839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4.0 g of 3,4-epoxy-1-(β,β,β-trichloroethoxycarbonyl)-pyrrolidine are dissolved in 15 ml of dioxane, and the solution is treated with 50 ml of 6 N hydrochloric acid. The slightly exothermic reaction is kept at room temperature by means of a water bath, and the reaction mixture is stirred for 15 hours, then diluted with water and extracted 3 times with 100 ml of methylene chloride. The organic phase is washed with 0.1 N sodium hydroxide solution and then with aqueous sodium chloride solution, dried over sodium sulphate and then evaporated to dryness, first under a water pump vacuum and then under a high vacuum, 3-hydroxy-4-chloro-1-(β,β,β-trichloroethoxycarbonyl)-pyrrolidine being obtained as a slightly yellow oil.

WORKUP

后处理

  1. customThe slightly exothermic reaction
  2. customis kept at room temperature by means of a water bath
  3. extractionextracted 3 times with 100 ml of methylene chloride
  4. washThe organic phase is washed with 0.1 N sodium hydroxide solution
  5. dry with materialwith aqueous sodium chloride solution, dried over sodium sulphate
  6. customevaporated to dryness, first under a water pump vacuum