反应详情

A mixture of tert-butyl piperidin-4-ylmethylcarbamate (Epsilon, 0.80 g, 3.73 mmol), (1R,2R)-2-phenylcyclopropanecarboxylic acid (T. Riley eta al, J. Med. Chem., 15, 1187, 1972) (0.61 g, 3.73 mmol), EDC (1.07 g, 5.60 mmol) and HOBt (0.76 g, 5.60 mmol) in DMF (10 mL) was stirred at RT for 2 h. The reaction mixture was diluted with ethyl acetate (200 mL), washed with aq. sat. NaHCO3 (50 mL), water (5×50 mL), brine (50 mL), dried over Na2SO4, filtered and concentrated. The residue was chromatographed on silica gel 60 (90 g), eluting with 10:1–10:89–80 CH2Cl2:2-propanol:hexane to give the title compound. (1.22 g, 91.0%). M.S. (M+1): 359.

1. washwashed with aq. sat. NaHCO3 (50 mL), water (5×50 mL), brine (50 mL)
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was chromatographed on silica gel 60 (90 g)
6. washeluting with 10:1–10:89–80 CH2Cl2