反应详情

温度

0 °C

To a solution of 4-hydroxy-1-methoxy-piperidine-4-carboxylic acid ethyl ester (1.0 g, 4.92 mmol) in 10 ml pyridine under argon was added 4-dimethylaminopyridine DMAP (30 mg, 0.25 mmol). The solution was cooled down to 0° C., then (2,5-dimethyl-phenyl)-acetyl chloride (0.99 g, 5.4 mmol) was added dropwise. The reaction mixture was warmed up to room temperature and left stirring for 5 days. Then the reaction mixture was concentrated and the crude product was purified by column chromatography on silica gel (ethyl acetate/cyclohexane first 1:15, then 1:9) to give pure 4-[2-(2,5-dimethyl-phenyl)-acetoxy]-1-methoxy-piperidine-4-carboxylic acid ethyl ester (compound P3.2) as light yellow oil. Yield: 530 mg.

1. temperatureThe reaction mixture was warmed up to room temperature
2. waitleft
3. concentrationThen the reaction mixture was concentrated
4. customthe crude product was purified by column chromatography on silica gel (ethyl acetate/cyclohexane first 1:15