反应详情

温度

130 °C

2-Amino-6-chloro-nicotinic acid methyl ester (2.95 g, 15.8 mmol), vinyl tri-n-butyltin (5.01 g, 15.8 mmol) and tetrakis(triphenylphosphine)palladium(0) (1.83 g, 1.58 mmol) were suspended in xylene (15 mL), and heated for 1 hour at 130° C. The reaction mixture was allowed to room temperature, water and ethyl acetate were added thereto, this mixture was filtered through Celite pad, then, the filtrate thereof was partitioned. The organic layer was separated, the solvent was evaporated in vacuo, and the residue was purified by silica gel column chromatography to obtain the title compound (1.87 g, 10.5 mmol, 66%) as a white solid.

1. customwas allowed to room temperature
2. filtrationthis mixture was filtered through Celite pad
3. customthe filtrate thereof was partitioned
4. customThe organic layer was separated
5. customthe solvent was evaporated in vacuo
6. customthe residue was purified by silica gel column chromatography