HRID52097

反应详情

EQUATION

反应方程式

HRID 52097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.38 g of 3-(4-piperidinomethyl-2-pyridyloxy)propylamine and 0.18 g of 1,4-oxathian-2-one was added to 10 ml of ethanol, and the resulting mixture was heated under reflux for 2 hours. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure. The concentrate was mixed with water, and the resulting aqueous mixture was extracted with ethyl acetate. The extract was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 1:9 by volume mixture of methanol and methylene chloride as the eluent, to give 0.49 g (yield 88%) of the title compound as an oil.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 2 hours
  3. concentrationAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
  4. additionThe concentrate was mixed with water
  5. extractionthe resulting aqueous mixture was extracted with ethyl acetate
  6. concentrationThe extract was concentrated by evaporation under reduced pressure
  7. customthe concentrate was purified by column chromatography through silica gel
  8. additionby volume mixture of methanol and methylene chloride as the eluent