反应详情

温度

80 °C

To a solution of 2,4-dichloro-5-fluoropyrimidine (1 g, 5.98 mmol) in isopropanol (18 mL, 3 mL/mmol) was added DIPEA (1.6 mL, 8.9 mmol) and 3-amino-N-methylbenzamide (900 mg, 5.98 mmol) and the mixture was heated at 80° C. for 7 h. The reaction mixture was concentrated under reduced pressure and extracted with EtOAc (2×40 mL) and water (2×40 mL). The organic extracts were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. Purification by column chromatography provided 3-((2-chloro-5-fluoropyrimidin-4-yl)amino)-N-methylbenzamide (800 mg, 50%) as a solid. Observed mass (M+1): 281.1

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionextracted with EtOAc (2×40 mL) and water (2×40 mL)
3. washThe organic extracts were washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customPurification by column chromatography