反应详情

A solution of 4-fluoro-2-methoxy-1-nitrobenzene (1.711 g, 10 mmol), N,N-dimethylpiperidin-4-amine (1.410 g, 11.00 mmol) and N-ethyl-N-isopropylpropan-2-amine (3.48 mL, 20.00 mmol) in anhydrous N,N-dimethylformamide (25 mL) was stirred at 70° C. overnight. The mixture was concentrated and the residue was mixed with water (60 mL), adjusted to pH 12, then extracted with CH2Cl2. The crude product was purified on a silica gel column eluting with 7.5% methanol in CH2Cl2 saturated with NH3 to provide the title compound. (ESI+) m/e 280.1 (M+H)+.

1. concentrationThe mixture was concentrated
2. additionthe residue was mixed with water (60 mL)
3. extractionextracted with CH2Cl2
4. customThe crude product was purified on a silica gel column
5. washeluting with 7.5% methanol in CH2Cl2 saturated with NH3