HRID1700681

反应详情

EQUATION

反应方程式

HRID 1700681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(2-chlorophenyl)-1-[2-(4-methylphenylsulfonyl)hydrazino]cyclohexen-3-one (2.0 g), 2-bromo-4′-chloroacetophenone (1.6 g), anhydrous potassium carbonate (1.8 g) and ethanol (50 ml) was refluxed for 13 hours. Under reduced pressure, the solvent was evaporated, and the residue was extracted with ethyl acetate. The organic layer was concentrated, and the residue was purified with silica gel column chromatography. The resulting crystals were recrystallized from ethyl acetate-hexane to give 7-(2-chlorophenyl)-4-(4-chlorophenyl)-5,6,7,8-tetrahydrocinnolin-5-one (0.2 g) as colorless crystals.

WORKUP

后处理

  1. temperaturewas refluxed for 13 hours
  2. customUnder reduced pressure, the solvent was evaporated
  3. extractionthe residue was extracted with ethyl acetate
  4. concentrationThe organic layer was concentrated
  5. customthe residue was purified with silica gel column chromatography
  6. customThe resulting crystals were recrystallized from ethyl acetate-hexane