HRID1700702

反应详情

EQUATION

反应方程式

HRID 1700702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-(5-chloro-2-fluorophenyl)cyclohexane-1,3-dione (2 g) and ammonium acetate (1.9 g) in ethanol (15 ml) was refluxed for 15 hours. The reaction solution was concentrated under reduced pressure, and to the residue were added water (30 ml) and ethyl acetate (150 ml). The mixture was shaken, and the separated upper layer was washed with water and concentrated under reduced pressure. The residue was washed with ethyl acetate and dried to give 1-amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one (1.45 g) as yellow crystals.

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionto the residue were added water (30 ml) and ethyl acetate (150 ml)
  3. washthe separated upper layer was washed with water
  4. concentrationconcentrated under reduced pressure
  5. washThe residue was washed with ethyl acetate
  6. customdried