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 solution of 1-(4-methoxycarbonylphenyl)-3,4-dihydrocarbostyril (1.84 g) in methanol (40 ml) is added a 5 aqueous sodium hydroxide solution (20 ml) and the mixture is stirred at room temperature overnight. Methanol is distilled off under reduced pressure and to the residue is added water. After the solution is washed with dichloromethane, the aqueous layer is made acidic with concentrated hydrochloric acid and extracted with diethyl ether and dried over magnesium sulfate. The solvent is distilled off under reduced pressure and the resulting residue is purified by silica gel column chromatography, followed by recrystallization from ethanol to give 1-(4-carboxyphenyl)-3,4-dihydrocarbostyril (0.87 g) as pale yellow powders, m.p. 265°-270° C.
WORKUP
后处理
- distillationMethanol is distilled off under reduced pressure and to the residue
- additionis added water
- washAfter the solution is washed with dichloromethane
- extractionextracted with diethyl ether
- dry with materialdried over magnesium sulfate
- distillationThe solvent is distilled off under reduced pressure
- customthe resulting residue is purified by silica gel column chromatography
- customfollowed by recrystallization from ethanol