反应详情

温度

90 °C

To 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)cyclopropanecarbonyl chloride (369 mg, 1.42 mmol) and 4-(6-methoxypyridin-3-yl)-5-methylpyrimidin-2-amine (153 mg, 0.71 mmol), pyridine (4 mL) was added. The reaction was heated at 90° C. for three and a half hours. The pyridine was evaporated under reduced pressure. The resulting mixture was dissolved in ethyl acetate and filtered. The filtrate was washed with saturated aqueous NaHCO3 (×3). The organic layer was dried over anhydrous Na2SO4 and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel to yield 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-N-(4-(6-methoxypyridin-3-yl)-5-methylpyrimidin-2-yl)cyclopropanecarboxamide. ESI-MS m/z calc. 440.13. Found 441.5 (M+1)+. Retention time 1.72 minutes.

1. customThe pyridine was evaporated under reduced pressure
2. dissolutionThe resulting mixture was dissolved in ethyl acetate
3. filtrationfiltered
4. washThe filtrate was washed with saturated aqueous NaHCO3 (×3)
5. dry with materialThe organic layer was dried over anhydrous Na2SO4
6. customevaporated under reduced pressure
7. customThe crude product was purified by column chromatography on silica gel