反应详情

To a solution of 2-bromomethyl-4-methoxy-benzoic acid methyl ester (1.28 g, 4.94 mmol, 1.0 equiv) in methanol (9 mL) and triethylamine (0.83 mL) was added 4-amino-piperidine-1-carboxylic acid tert-butyl ester (1.04 g, 5.19 mmol, 1.05 equiv; commercially available) and the reaction stirred at rt overnight. The reaction mixture was poured on crashed ice/diluted HCl, extracted with ethyl acetate, the combined organic phases washed with a sat. solution of NaHCO3 and water, dried over Na2SO4 and concentrated by evaporation under reduced pressure. The crude material was purified with silica column chromatography eluting with hexane/ethyl acetate (3:7) yielding 0.84 g (49%) of the title compound as white crystals. MS (ISP): 347.3 [M+H]+.

1. additionThe reaction mixture was poured
2. extractionextracted with ethyl acetate
3. washthe combined organic phases washed with a sat. solution of NaHCO3 and water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated by evaporation under reduced pressure
6. customThe crude material was purified with silica column chromatography
7. washeluting with hexane/ethyl acetate (3:7)