HRID1354094

反应详情

EQUATION

反应方程式

HRID 1354094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-methyl-2-phenylcyclohexanone (4.7 g, 25 mmol) from Preparation 3 above, and sodium hydride (1.1 g of 60% dispersion in mineral oil, 28 mmol) in 15 mL of dimethyl carbonate and 75 mL of benzene, was heated under reflux for 4 h. The mixture was cooled to room temperature and poured into dilute ice-cold aqueous HCl. The organic layer was washed with brine, dried (sodium sulfate) and evaporated to afford 6.36 g of 3-methyl-2-oxo-3-phenyl-cyclohexanecarboxylic acid methyl ester as an oil.

WORKUP

后处理

  1. customfrom Preparation 3 above
  2. temperatureunder reflux for 4 h
  3. additionpoured into dilute ice-cold aqueous HCl
  4. washThe organic layer was washed with brine
  5. dry with materialdried (sodium sulfate)
  6. customevaporated