HRID974962

反应详情

EQUATION

反应方程式

HRID 974962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(2-carbamoyl-2,2-diphenylethyl)piperidine (300 mg, 0.97 mmol) (Preparation 3), phenethyl bromide (198 mg, 1.07 mmol) and potassium carbonate (400 mg) in acetonitrile (10 ml) was heated under reflux for 6 hours, allowed to cool to room temperature and evaporated. The residue was partitioned between dichloromethane and 10% aqueous potassium carbonate solution and the aqueous layer was extracted twice into dichloromethane. The combined organic layers were dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-10% methanol as eluant. Appropriate fractions were combined and evaporated to give the title compound (195 mg, 49%) as a colourless foam, which was characterised as a hydrate.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. customevaporated
  4. customThe residue was partitioned between dichloromethane and 10% aqueous potassium carbonate solution
  5. extractionthe aqueous layer was extracted twice into dichloromethane
  6. dry with materialThe combined organic layers were dried over magnesium sulphate
  7. customevaporated
  8. customThe residue was purified by chromatography on silica
  9. customevaporated