HRID1719545

反应详情

EQUATION

反应方程式

HRID 1719545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled solution of sodium (3.25 g) in ethanol (75 ml) was added a solution of ethyl β-(2-hydroxy-4-pyridyl)propionate (25.38 g) in ethanol (150 ml). This mixture was stirred for 45 minutes and then benzyl chloride (16.58 g) in ethanol (125 ml) was added. The reaction mixture was stirred under reflux for 9 hours, allowed to cool and evaporated under reduced pressure. The residue was taken up in water (150 ml) and diethyl ether (150 ml), the aqueous layer was separated and washed with diethyl ether (2×120 ml). The combined ether extracts were washed with water, dried over MgSO4 and evaporated under reduced pressure to yield ethyl β-(N-benzyl-2-oxo-4-pyridyl)propionate (30.29 g) as an oil.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred
  2. temperatureunder reflux for 9 hours
  3. temperatureto cool
  4. customevaporated under reduced pressure
  5. customdiethyl ether (150 ml), the aqueous layer was separated
  6. washwashed with diethyl ether (2×120 ml)
  7. washThe combined ether extracts were washed with water
  8. dry with materialdried over MgSO4
  9. customevaporated under reduced pressure