HRID37510

反应详情

EQUATION

反应方程式

HRID 37510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.28 g of sodium sulfite in 7 ml of water was added to a solution of 0.70 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine in 7 ml of ethanol, and the mixture was heated under reflux for minutes. After the reaction mixture was concentrated, the concentrate was acidified with 1N HCl, followed by extraction with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over magnesium sulfate. After concentration to dryness under reduced pressure, the residue was recrystallized from chloroform/ether, to give 0.47 g of white crystals.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for minutes
  3. concentrationAfter the reaction mixture was concentrated
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationAfter concentration to dryness under reduced pressure
  8. customthe residue was recrystallized from chloroform/ether