反应详情

温度

80 °C

A mixture of 4-chloro-3-nitropyridine (580 mg, 3.6 mmol), tert-butyl [(3S,5R)-5-(trifluoromethyl)piperidin-3-yl]carbamate (800 mg, 3 mmol), isopropyl alcohol (5.0 mL) and DIPEA (1.0 mL, 6.0 mmol) was stirred at 80° C. overnight. The reaction mixture was concentrated under reduced pressure and the residue was purified by column chromatography on silica gel using CombiFlash® apparatus eluting with 50-100% EtOAc/hexanes. The purification gave 1.0 g (80% yield) of the sub-title compound as a yellow solid. LCMS calc. for C16H22F3N4O4(M+H)+: m/z=: 391.2. found: 391.1.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe residue was purified by column chromatography on silica gel using CombiFlash® apparatus
3. washeluting with 50-100% EtOAc/hexanes
4. customThe purification