HRID1700644

反应详情

EQUATION

反应方程式

HRID 1700644 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 (1.56 g), anhydrous potassium carbonate (0.72 g), 1-bromobutan-2-one (0.785 g) and methanol (30 ml) was stirred at room temperature for 2.5 hours. To the mixture was added anhydrous potassium carbonate (0.72 g), and the mixture was stirred at room temperature 1.5 hours and refluxed for 30 minutes. 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 to give 7-(2-chlorophenyl)-4-ethyl-5,6,7,8-tetrahydrocinnolin-5-one (0.492 g) as oil.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature 1.5 hours
  2. temperaturerefluxed for 30 minutes
  3. customUnder reduced pressure, the solvent was evaporated
  4. extractionthe residue was extracted with ethyl acetate
  5. concentrationThe organic layer was concentrated
  6. customthe residue was purified with silica gel column chromatography