反应详情

温度

70 °C

To a solution added of nipecotic acid (8.0 g, 61.9 mmol) in N,N-dimethylformamide (80 mL) is benzyl bromide (31.8 g, 186 mmol) and potassium carbonate (42.8 g, 310 mmol). The mixture is heated at 70° C. for 18 hours and diluted with ethyl acetate and water. The organic extract is washed with 1.0 M hydrochloric acid, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue is purified by column chromatography (1:7 ethyl acetate/hexanes) to afford the title compound (8.6 g). 1H NMR (200 MHz, DMSO-d6): δ 7.27–7.42 (m, 10H), 5.07 (s, 2H), 3.45 (s, 2H), 2.88–2.49 (m, 3H), 2.32–1.32 (m, 6H).

1. extractionThe organic extract
2. washis washed with 1.0 M hydrochloric acid, water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue is purified by column chromatography (1:7 ethyl acetate/hexanes)