HRID1894849

反应详情

EQUATION

反应方程式

HRID 1894849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.4 ml (15.3 mmol) of aniline (starting product 1) are added to a solution of 1.3 ml (12.5 mmol) of cyclohexanone (starting product 2) in 20 ml of acetic acid at 0° C. The solution is stirred for a time and 1.9 ml (14.2 mmol) of trimethylsilyl cyanide are added. The reaction medium is stirred for one night at room temperature. It is then poured gently into an ice-cold ammonium hydroxide solution until the pH is basic and extracted with dichloromethane. The organic phases are collected and washed with water. They are dried over sodium sulfate. The residue is precipitated in dichloromethane and heptane. The solid is filtered and dried. 2.2 g of 1-phenylaminocyclohexanecarbonitrile are obtained in the form of a whitish solid. M.p.=67-9° C., yield=88%.

WORKUP

后处理

  1. additionare added
  2. extractionextracted with dichloromethane
  3. customThe organic phases are collected
  4. washwashed with water
  5. dry with materialThey are dried over sodium sulfate
  6. customThe residue is precipitated in dichloromethane
  7. filtrationThe solid is filtered
  8. customdried