HRID224375

反应详情

EQUATION

反应方程式

HRID 224375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4.22 g (0.032 m) of 5-methyl-4-oximino-1,3-oxathiolane and 5.0 g (0.032 m) of N-methyl-N-(methylthiosulfenyl) carbamoyl fluoride in 25 ml of dioxane was added 3.25 g (0.032 m) of triethylamine. After stirring at room temperature for 19 hrs. the reaction mixture was quenched with 100 ml of water and extracted in ethyl acetate. After the usual work-up it yielded a residual oil. Addition of isopropyl ether resulted in the precipitation of 0.16 g of a solid biscarbamate. The concentrated filtrate was purified by column chromatography to yield 2.97 g of an oil.

WORKUP

后处理

  1. customthe reaction mixture was quenched with 100 ml of water
  2. extractionextracted in ethyl acetate
  3. customAfter the usual work-up it yielded a residual oil