HRID1666724

反应详情

EQUATION

反应方程式

HRID 1666724 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 are added to a solution of 1.3 ml (12.5 mmol) of cyclohexanone in 20 ml of acetic acid at 0° C. The solution is stirred for 10 minutes and 1.9 ml (14.2 mmol) of trimethylsilyl cyanide are added. The reaction medium is stirred overnight at room temperature. It is then gently poured into a solution of ice-cold ammonium hydroxide, while keeping the pH 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 whitish crystals. Yield=88%, m.p.=67-9° C.

WORKUP

后处理

  1. stirringThe reaction medium is stirred overnight at room temperature
  2. additionIt is then gently poured into a solution of ice-cold ammonium hydroxide
  3. extractionextracted with dichloromethane
  4. customThe organic phases are collected
  5. washwashed with water
  6. dry with materialThey are dried over sodium sulfate
  7. customThe residue is precipitated in dichloromethane
  8. filtrationThe solid is filtered
  9. customdried