HRID344772

反应详情

EQUATION

反应方程式

HRID 344772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4-azido-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran (0.92g) in acetone (20 ml) was added concentrated hydrochloric acid (3 ml) and zinc dust (0.6g) in portions, with vigorous stirring. After 15 min the reaction was diluted with water, filtered and the filtrate extracted with ethyl acetate. The aqueous phase was made basic with 10% (w/v) aqueous sodium hydroxide solution and further extracted with ethyl acetate. The combined organic phase was dried over anhydrous sodium sulphate, filtered and the solvent evaporated in vacuo to give the title compound (0.69g).

WORKUP

后处理

  1. filtrationfiltered
  2. extractionthe filtrate extracted with ethyl acetate
  3. extractionfurther extracted with ethyl acetate
  4. dry with materialThe combined organic phase was dried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. customthe solvent evaporated in vacuo