HRID2399698

反应详情

EQUATION

反应方程式

HRID 2399698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.0 g of 7-hydroxy-1,2-benzisothiazole are dissolved in 20 ml of THF, and 460 mg of sodium hydride (60%) are added to the mixture at 0° C. When the evolution of gas has ended, 1 ml of allyl bromide is added dropwise, the reaction mixture is stirred for one day at room temperature. Again, 1 ml of allyl bromide and 40 mg of sodium hydride are added, and the mixture is stirred for 2 days under reflux. The reaction mixture is poured into water, rendered basic using 1 N potassium hydroxide solution and extracted using ethyl acetate. The organic phase is washed with saline, dried over sodium sulfate, filtered and concentrated. Silica gel chromatography with ethyl acetate/hexane (1:5) as mobile phase gives 2.0 g of 7-allyloxy-1,2-benzisothiazole; nD20 =1.6039 .

WORKUP

后处理

  1. stirringthe mixture is stirred for 2 days
  2. temperatureunder reflux
  3. extractionextracted
  4. washThe organic phase is washed with saline
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated