反应详情

温度

90 °C

To 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-N-(6′-methoxy-4,5′-dimethyl-2,3′-bipyridin-6-yl)cyclopropanecarboxamide (0.075 g, 0.165 mmol) in 1,4-dioxane (2 mL) was added aqueous 4 M HCl (447 μL, 1.79 mmol) drop-wise. The reaction was stirred at 90° C. for 1.5 hours. The reaction was allowed to cool down to room temperature and then quenched with Et3N. The solvent was evaporated under reduced pressure. The crude compound was dissolved in ethyl acetate and washed with water (2×) and brine (1×). The organic layer was dried over Na2SO4, filtered and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel (0-100% ethyl acetate in hexane) to yield 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-N-(4-methyl-6-(5-methyl-6-oxo-1,6-dihydropyridin-3-yl)pyridin-2-yl)cyclopropanecarboxamide as a white solid (33 mg, 46%); ESI-MS m/z calc. 439.41. found 440.5 (M+1)+. Retention time 1.72 minutes.

1. temperatureto cool down to room temperature
2. customquenched with Et3N
3. customThe solvent was evaporated under reduced pressure
4. dissolutionThe crude compound was dissolved in ethyl acetate
5. washwashed with water (2×) and brine (1×)
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. customevaporated under reduced pressure
9. customThe crude product was purified by column chromatography on silica gel (0-100% ethyl acetate in hexane)