HRID1112407

反应详情

EQUATION

反应方程式

HRID 1112407 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 4.0 g (0.024 m) of 2,2-dimethyl-2,3-dihydrobenzofuran-7-ol and 6.56 g (0.024 m) of N-methyl-N-(p-tert-butylphenylthiosulfenyl)carbamoyl fluoride in 25 ml of dioxane was added 2.45 g (0.024 m) of triethylamine. After 24 hours the reaction mixture was diluted with 200 ml of water and the product was extracted in ethylacetate. The organic extract was washed in turn with diluted sodium hydroxide and water, dried over MgSO4 and concentrated under reduced pressure. The product was crystallized from isopropyl ether to yield 4.0 g of a white solid, m.p. 150°-151° C.

WORKUP

后处理

  1. extractionthe product was extracted in ethylacetate
  2. extractionThe organic extract
  3. washwas washed in turn with diluted sodium hydroxide and water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe product was crystallized from isopropyl ether