反应详情

温度

100 °C

To 5-nitropyrimidin-2-amine (1.0 g, 7.1 mmol) in pyridine (10 mL) was added 3-chloro-4-fluorobenzoic acid (1.7 g, 9.7 mmol). The reaction mixture was heated at 100° C. for 4 hrs and allowed to cool to rt. 15 mL H2O was added. A precipitate was collected by filtration and purified by silica gel chromatography, eluting with CH2Cl2 followed by 10% EtOAc/CH2Cl2 to give 1.16 g (55% yield) 1C. RP HPLC ret. t.: 2.22 min. and (M+H)+: 297.

1. temperatureto cool to rt
2. filtrationA precipitate was collected by filtration
3. custompurified by silica gel chromatography
4. washeluting with CH2Cl2