HRID1980106

反应详情

EQUATION

反应方程式

HRID 1980106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1.4 g of N-methyl-N-(2-chloromethyl-2-propanesulfenyl)carbamoyl chloride and 0.966 g of 2-oximino-1,4-dithiane in 50 ml of dioxane, was added dropwise with stirring 0.76 g of triethylamine. After allowing the reaction mixture to stand at ambient temperature for 16 hours it was diluted with water and extracted into ethylacetate. The organic extract was washed with water, dried over sodium sulfate and concentrated under reduced pressure. The product was crystallized from isopropyl ether-methylene chloride solution. The weight of first crop was 1.0 g. m.p. 116°-117° C.

WORKUP

后处理

  1. extractionextracted into ethylacetate
  2. extractionThe organic extract
  3. washwas washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe product was crystallized from isopropyl ether-methylene chloride solution