HRID1501281
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To the solution of ethyl 1-benzoyl-3,5-dimethyl-2-oxo-1,2-dihydropyridine-4-carboxylate (1.06 g, 3.54 mmol) in methanol/H2O (40 mL, 1:1) was added KOH (0.79 g, 14.16 mmol). The mixture was refluxed overnight. Then the mixture was concentrated under vacuum, diluted with water (5 mL) and acidified with 1 N HCl to pH=2. The mixture was extracted with ethyl acetate. The extractions were combined, dried over Na2SO4, and concentrated to give a residue 3,5-dimethyl-2-oxo-1-(1-phenylethyl)-1,2-dihydropyridine-4-carboxylic acid as a white solid. (70 mg, yield 7.3%) LRMS (M+H+) m/z: calcd 271.31. found 272.1. The residue was used in the next step.
WORKUP
后处理
- temperatureThe mixture was refluxed overnight
- concentrationThen the mixture was concentrated under vacuum
- additiondiluted with water (5 mL)
- extractionThe mixture was extracted with ethyl acetate
- extractionThe extractions
- dry with materialdried over Na2SO4
- concentrationconcentrated