反应详情

温度

40 °C

A vial was charged with perfluorophenyl 1-chloroisoquinoline-6-sulfonate (From Step 1 in Example 73; 0.050 g, 0.122 mmol), (5,6-dichloro-2-methoxypyridin-3-yl)boronic acid (0.030 g, 0.134 mmol), potassium carbonate (0.051 g, 0.366 mmol), and Pd(Ph3P)4 (0.014 g, 0.012 mmol). The vial was flushed with Ar (g), then dioxane (0.915 ml) and water (0.305 ml) were added. The reaction was heated at 40° C. for one hour. The reaction was diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were dried with sodium sulfate, filtered, and concentrated. The material was purified via column chromatography (RediSep Gold 12 g, gradient elution 0-50% EtOAc:Heptane) to afford perfluorophenyl 1-(5,6-dichloro-2-methoxypyridin-3-yl)isoquinoline-6-sulfonate as a white solid. (ESI) 551.0 (M+H)+.

1. customThe vial was flushed with Ar (g)
2. additiondioxane (0.915 ml) and water (0.305 ml) were added
3. additionThe reaction was diluted with ethyl acetate
4. washwashed with water
5. extractionThe aqueous layer was extracted with ethyl acetate
6. dry with materialthe combined organic layers were dried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe material was purified via column chromatography (RediSep Gold 12 g, gradient elution 0-50% EtOAc:Heptane)