反应详情

To a solution of methyl 5-bromo-2-chloronicotinate (170 mg, 0.68 mmol) in 3 mL of DMSO was added CsF (152 mg, 1.0 mmol). The solution was stirred at room temperature for 2 d and then heated at 60° C. for 4 h. After cooling, the mixture was diluted with 30 mL of H2O. The aqueous solution was extracted with EtOAc and the combined organic layers were washed with brine, and dried over MgSO4. After filtration and concentration in vacuo, the residue was purified by silica gel flash chromatography to give the desired product (90 mg, 57% yield). MS (ESI+) m/z 234.06, 236.09 (M+H)+.

1. temperatureheated at 60° C. for 4 h
2. temperatureAfter cooling
3. extractionThe aqueous solution was extracted with EtOAc
4. washthe combined organic layers were washed with brine
5. dry with materialdried over MgSO4
6. filtrationAfter filtration and concentration in vacuo
7. customthe residue was purified by silica gel flash chromatography