反应详情

温度

90 °C

To 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-N-(6′-methoxy-4,4′-dimethyl-2,3′-bipyridin-6-yl)cyclopropanecarboxamide (38 mg, 0.083 mmol) in 1,4-dioxane (1.5 mL) was added aqueous 4 M HCl (225 μL, 0.899 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 (0-10% methanol in dichloromethans) to yield 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-N-(4-methyl-6-(4-methyl-6-oxo-1,6-dihydropyridin-3-yl)pyridin-2-yl)cyclopropanecarboxamide as a white solid (7 mg, 19%). ESI-MS m/z calc. 439.41. found 440.5 (M+1)+. Retention time 1.60 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 (0-10% methanol in dichloromethans)