反应详情

温度

60 °C

0.370 g of 2-methyl-2-piperidin-3(R,S)-yl-propionic acid methyl ester hydrochloride are dissolved in 0.5 ml of 3M NaOH. 2 ml of formic acid and 0.19 ml of formaldehyde (35% aqueous solution) are added and the reaction solution is warmed to 60° C. for 20 hours. The solution is cooled to room temperature, neutralised with 3M NaOH to pH 8-9 and extracted with dichloromethane (3×10 ml). The combined organic phases are washed with water (10 ml), dried over sodium sulphate and concentrated by evaporation. The residue is purified by means of flash chromatography (SiO2 60F) to provide the title compound as a colourless oil. Rf 0.19 (200:20:1 dichloromethane-methanol-25% conc. ammonia).

1. temperatureThe solution is cooled to room temperature
2. extractionextracted with dichloromethane (3×10 ml)
3. washThe combined organic phases are washed with water (10 ml)
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated by evaporation
6. customThe residue is purified by means of flash chromatography (SiO2 60F)