反应详情

温度

80 °C

Half of the solution prepared in Step 3 and 4-bromo-2-(tert-butyldimethylsilyloxy)-6-methylpyridine (30 mg, 0.10 mmol) are mixed and diluted with dioxane (0.15 mL). KOAc (15 mg, 0.15 mmol) and Pd(dppf)Cl2DCM (2 mg, 0.0025 mmol) are added and the system is flushed with N2 and heated at 80° C. for 2.5 h. The mixture is cooled to rt, diluted with DCM (5 mL) and MeOH (1 mL) and filtered through celite. The solvents are evaporated, the residue is suspended in DCM (2 mL) and TFA (0.5 mL) is added, causing the solid to dissolve. The solution is stirred at rt overnight and the solvents are then evaporated. The residue is purified by preparative HPLC to afford the title compound as a yellow solid. LCMS: Rt=0.84 min (100%), m/z (ESI) 403 (M+H)+.

1. customthe system is flushed with N2
2. temperatureThe mixture is cooled to rt
3. additiondiluted with DCM (5 mL) and MeOH (1 mL)
4. filtrationfiltered through celite
5. customThe solvents are evaporated
6. additionTFA (0.5 mL) is added
7. dissolutionto dissolve
8. customthe solvents are then evaporated
9. customThe residue is purified by preparative HPLC