反应详情

温度

135 °C

A mixture of diethyl 2-propyl-6-vinylpyridine-3,5-dicarboxylate (9.00 g), tert-butyl 4-aminopiperidine-1-carboxylate (7.42 g) and N-ethyl-N-isopropylpropan-2-amine (8.09 mL) in DMA (45 mL) was stirred at 130 to 140° C. for 4.5 hours. The mixture was poured into water at room temperature and extracted with ethyl acetate. The organic layer was separated, washed with brine twice, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was passed through a silica gel-pad (hexane/ethyl acetate), and concentrated in vacuo. The residue was purified by a silica gel column chromatography (hexane/ethyl acetate) to give the title compound (10.0 g).

1. extractionextracted with ethyl acetate
2. customThe organic layer was separated
3. washwashed with brine twice
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated in vacuo
6. concentrationconcentrated in vacuo
7. customThe residue was purified by a silica gel column chromatography (hexane/ethyl acetate)