HRID924624

反应详情

EQUATION

反应方程式

HRID 924624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25 g 2,2-Dimethyl-malonic acid diethyl ester, 7.8 g potassium hydroxide and 500 ml ethanol were mixed in a round-bottomed flask and refluxed for 3 hours. Then again 2.2 g potassium hydroxide were added and the mixture was refluxed overnight. The solvent was removed on a rotovap, 250 ml H2O were added and the mixture was washed with ether. The aqueous phase was acidified with HCl to pH 3-4 followed by two extractions with dichloromethane. The organic solvent was dried and evaporated and the resulting product was characterized by 1H-NMR.

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. temperaturethe mixture was refluxed overnight
  3. customThe solvent was removed on a rotovap, 250 ml H2O
  4. additionwere added
  5. washthe mixture was washed with ether
  6. extractionfollowed by two extractions with dichloromethane
  7. customThe organic solvent was dried
  8. customevaporated