反应详情

温度

20 °C

A mixture of (R)-methyl 2-oxo-1-(1-phenylethyl)-1,2-dihydropyridine-4-carboxylate (451 mg, 1.75 mmol), lithium hydroxide monohydrate (369 mg, 8.77 mmol), water (4 mL) and methanol (4 mL) in tetrahydrofuran (12 mL) was stirred at 20° C. for 12 hours. The reaction mixture was concentrated. The residue was acidified with concentrated hydrochloride solution to pH=2. The mixture was extracted with ethyl acetate (20 mL×2). The organic phase was dried over sodium sulfate and filtered. The filtrate was concentrated. The residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=1:2) to give (R)-2-oxo-1-(1-phenylethyl)-1,2-dihydropyridine-4-carboxylic acid as a white solid (336 mg, 80%). LRMS (M+H+) m/z: calcd 243.13. found 243.

1. concentrationThe reaction mixture was concentrated
2. extractionThe mixture was extracted with ethyl acetate (20 mL×2)
3. dry with materialThe organic phase was dried over sodium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated
6. customThe residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=1:2)