HRID2107094

反应详情

EQUATION

反应方程式

HRID 2107094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a mixture of 0.30 g of 4-acetyl-3-hydroxy-2-propylbenzyl chloride, 0.22 g of 2-amino-5-mercapto-1,3,4-thiadiazole, 0.22 g of anhydrous potassium carbonate and 3 ml of methyl ethyl ketone were added catalytic amounts of potassium iodide and tetra-n-butylammonium bromide followed by stirring at 60° C. for 2 hours. Ethyl acetate was added to the reaction mixture. After insoluble matters were filtered off, the filtrate was washed with an aqueous sodium hydroxide solution and then dried over anhydrous magnesium sulfate The solvent was then removed by distillation to give 0.44 g of 2-amino-5-[(4-acetyl-3-hydroxy-2-propylbenzyl)thio]-1,3,4-thiadiazole.

WORKUP

后处理

  1. filtrationAfter insoluble matters were filtered off
  2. washthe filtrate was washed with an aqueous sodium hydroxide solution
  3. dry with materialdried over anhydrous magnesium sulfate The solvent
  4. customwas then removed by distillation