HRID440317

反应详情

EQUATION

反应方程式

HRID 440317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ammonium dithiocarbamate (1.4 g, 12.4 mmol) in 25 mL of ethanol was added 2-bromocyclohexanone (2.2 g, 12.4 mmol). The reaction was stirred at rt overnight. The next morning the reaction was heated at 70° C. for 1 h. The solvent was removed under reduced pressure. The product was subjected to flash chromatography (3:1 hexane/ethyl acetate) to recover a yellow solid. Recrystallization from ethyl acetate afforded 0.54 g of 2-mercapto-4,5,6,7-tetrahydrobenzothiazole.

WORKUP

后处理

  1. temperatureThe next morning the reaction was heated at 70° C. for 1 h
  2. customThe solvent was removed under reduced pressure
  3. customto recover a yellow solid
  4. customRecrystallization from ethyl acetate