HRID37510
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureunder reflux for minutes
- concentrationAfter the reaction mixture was concentrated
- extractionfollowed by extraction with ethyl acetate
- washThe extract was washed with an aqueous solution of sodium chloride
- dry with materialdried over magnesium sulfate
- concentrationAfter concentration to dryness under reduced pressure
- customthe residue was recrystallized from chloroform/ether