反应详情

(4-Amino-3-fluorophenyl)(piperazin-1-yl)methanone (2.74 mmol, 0.612 g), 3-(chloromethyl)-N-(1-cyano-1-cyclopropylethyl)benzamide (2.74 mmol, 0.72 g), sodium iodide (0.548 mmol, 0.082 g) and potassium carbonate (8.22 mmol, 1.136 g) were combined in acetonitrile (25 mL) and heated to reflux for 2 hours. The reaction was concentrated under reduced pressure and the resulting residue taken up in dichloromethane and washed with water. The organic phase was dried over sodium sulfate and concentrated under vacuum. The residue was purified by silica column chromatography (eluting with dichloromethane to 4% methanol/dichloromethane) to afford the title compound (195 mg). MS (ESI) m/z 450.3 [M+H]+

1. temperatureheated
2. temperatureto reflux for 2 hours
3. concentrationThe reaction was concentrated under reduced pressure
4. washwashed with water
5. dry with materialThe organic phase was dried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customThe residue was purified by silica column chromatography (eluting with dichloromethane to 4% methanol/dichloromethane)