反应详情

温度

60 °C

To a solution of 4-oxo-piperidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-ethyl ester (73.36 g, 0.27 mol) in DMF (734 mL) lithium carbonate (50 g, 0.676 mol) was added, followed by benzyl bromide (55.44 g, 0.324 mol). The mixture was heated to about 60° C. and stirred for about 20 hours. The reaction mixture was then cooled to room temperature and extracted with IPE, washed with water and dried over magnesium sulfate. After filtration and concentration in vacuo a solid was obtained. Recrystallization of the crude product in hexane afforded a white solid (33.6 g, yield 38.2%).

1. temperatureThe reaction mixture was then cooled to room temperature
2. extractionextracted with IPE
3. washwashed with water
4. dry with materialdried over magnesium sulfate
5. filtrationAfter filtration and concentration in vacuo a solid
6. customwas obtained
7. customRecrystallization of the crude product in hexane