HRID1699444

反应详情

EQUATION

反应方程式

HRID 1699444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 5.9 g (3 mmol) of 3,3-dimethyl-2,3-dihydro-1,2-benzoisothiazole 1,1-dioxide in 150 ml of DMF at room temperature was, after addition of 3.7 g (3.3 mmol) of potassium t-butoxide, heated under nitrogen to 80° C. Then 14.2 g (9 mmol) of 1-bromo-3-chloropropane were rapidly added and the mixture was stirred at 100° C. for 30 min. Pouring into ice-water was followed by extraction with ether, and the organic phases were washed with water, dried with sodium sulfate and then evaporated so that the product resulted as crystals which could be filtered off with suction. 6.7 g (82%) of substance were obtained. Melting point 107° C.

WORKUP

后处理

  1. customat room temperature
  2. extractionwas followed by extraction with ether
  3. washthe organic phases were washed with water
  4. dry with materialdried with sodium sulfate
  5. customevaporated so that the product
  6. customresulted as crystals which
  7. filtrationcould be filtered off with suction
  8. custom6.7 g (82%) of substance were obtained