反应详情

温度

100 °C

A mixture of N-(7-(6-chloro-4-methylpyridin-3-yl)isoquinolin-3-yl)cyclopropanecarboxamide (50 mg, 0.1 mmol), palladium acetate (2 mg, 0.007 mmol), 1,3-bis(dicyclohexylphosphino)propane bis(tetrafluoroborate) (9 mg, 0.014 mmol), potassium carbonate (29 mg, 0.21 mmol), methanol (0.1 mL), and N,N-dimethylformamide (1 mL) was purged with nitrogen and evacuated (3×), flushed with carbon monoxide and evacuated (2×), and then left under a carbon monoxide balloon and heated at 100° C. for 2 hours. The cooled reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (100 mL). The organic layer was separated, dried over sodium sulfate, filtered, and evaporated in vacuo to afford a residue that was purified by flash chromatography (silica, 4 g, ISCO, 0-60% ethyl acetate in heptane) to afford the title compound as a white solid (40 mg, 70%), which was used in the next step without further purification.

1. customwas purged with nitrogen
2. customevacuated (3×)
3. customflushed with carbon monoxide
4. customevacuated (2×)
5. waitleft under a carbon monoxide balloon
6. customThe cooled reaction mixture
7. washwashed with water (100 mL)
8. customThe organic layer was separated
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. customevaporated in vacuo
12. customto afford a residue that
13. customwas purified by flash chromatography (silica, 4 g, ISCO, 0-60% ethyl acetate in heptane)