HRID5032

反应详情

EQUATION

反应方程式

HRID 5032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

295.5 g (2.1 mol) of benzoyl chloride were added dropwise over the course of 10 minutes to a solution of 165.0 g (2.2 mol) of ammonium thiocyanate in 500 ml of absolute acetone. After refluxing for 10 minutes, 198.9 g (2.0 mol) of cyclohexylamine were added dropwise, and the mixture was refluxed for a further 20 minutes. It was then stirred into 4 1 of ice-water, and the water was decanted off the oily product. The residue was dissolved in a hot mixture of 2 1 of 10% strength sodium hydroxide solution and 500 ml of ethanol and refluxed for 30 minutes. The reaction mixture was then diluted with ice-water, and the pH was adjusted initially to 1 with concentrated hydrochloric acid and then to 9 with solid sodium bicarbonate. The resulting precipitate was filtered off with suction, washed with water and dried at 80° C. under reduced pressure.

WORKUP

后处理

  1. temperatureAfter refluxing for 10 minutes
  2. temperaturethe mixture was refluxed for a further 20 minutes
  3. customthe water was decanted off the oily product
  4. dissolutionThe residue was dissolved in a hot mixture of 2 1 of 10% strength sodium hydroxide solution and 500 ml of ethanol
  5. temperaturerefluxed for 30 minutes
  6. additionThe reaction mixture was then diluted with ice-water
  7. filtrationThe resulting precipitate was filtered off with suction
  8. washwashed with water
  9. customdried at 80° C. under reduced pressure