HRID374825
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
To a mixture of 217 g of 4-carboxybutyl-triphenylphosphonium bromide and 154 g of potassium tert.butoxide in 1.8 liters of tetrahydrofuran are added, at -25° C., 94 g of 3-acetylaminophenyl-3-pyridyl ketone. After 2 hours stirring at ambient temperature the reaction mixture is combined with 200 ml of water and then substantially evaporated down. The residue is taken up in 500 ml of water and washed with ethyl acetate. The aqueous phase is then neutralised by the addition of citric acid and extracted with ethyl acetate. The organic phase is evaporated down and the residue is recrystallised from ethyl acetate/acetone.
WORKUP
后处理
- additionare added, at -25° C.
- customsubstantially evaporated down
- washwashed with ethyl acetate
- additionThe aqueous phase is then neutralised by the addition of citric acid
- extractionextracted with ethyl acetate
- customThe organic phase is evaporated down
- customthe residue is recrystallised from ethyl acetate/acetone