HRID1700508

反应详情

EQUATION

反应方程式

HRID 1700508 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-(2-chlorophenyl)cyclohexane-1,3-dione (2.5 g) and ammonium acetate (2.6 g) in ethanol (50 ml) was refluxed for 12 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added sodium hydrogen carbonate solution. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and saturated brine, and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated to give crystals, which were recrystallized from ethyl acetate-hexane to give pale yellow crystals of 1-amino-5-(2-chlorophenyl)cyclohexen-3-one (2.2 g).

WORKUP

后处理

  1. customUnder reduced pressure, the solvent was evaporated
  2. additionto the residue was added sodium hydrogen carbonate solution
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe organic layer was washed with water and saturated brine
  5. dry with materialdried with magnesium sulfate
  6. customUnder reduced pressure, the solvent was evaporated
  7. customto give crystals, which
  8. customwere recrystallized from ethyl acetate-hexane