HRID2308760

反应详情

EQUATION

反应方程式

HRID 2308760 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 17.2 g of 2-bromo-4'-ethylpropiophenone, 12.5 g of 4-benzylpiperidine and 9.9 g of potassium carbonate in 250 ml of dry ethanol is heated under reflux for 4 hours, with stirring. The inorganic product is filtered off and washed with ethanol and the alcohol phase is concentrated in vacuo. The oily residue is taken up in diethyl ether and the mixture is extracted twice with dilute hydrochloric acid. After it has been rendered clearly alkaline with sodium hydroxide, the acid aqueous phase is then extracted three times with ethyl acetate. The organic phases are combined, washed with water until the washings are neutral, dried and evaporated in vauco. This give 19.15 g of an oily residue.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 4 hours
  3. filtrationThe inorganic product is filtered off
  4. washwashed with ethanol
  5. concentrationthe alcohol phase is concentrated in vacuo
  6. extractionthe mixture is extracted twice with dilute hydrochloric acid
  7. extractionthe acid aqueous phase is then extracted three times with ethyl acetate
  8. washwashed with water until the washings
  9. customdried
  10. customevaporated in vauco