反应详情

温度

110 °C

Methyl 6-bromo-2-pyridinecarboxylate (1) (5.0 g, 23.1 mmol), sodium acetate (5.7 g, 3.0 eq), tris-O-tolylphosphine (0.7 g, 2.3 mmol), allylpalladium chloride dimer (0.34 g, 0.93 mmol) and tert-butyl acrylate (3.6 g, 1.2 eq) are mixed in toluene (25 ml), and the resulting slurry is heated under a nitrogen atmosphere at 110° C. for approximately 12-16 hours. After cooling to ambient temperature, the precipitate is removed by filtration, and rinsed with ethyl acetate. The filtrate is washed with 1 M aqueous citric acid, water, and brine, and then dried with MgSO4 and filtered. The solvent is removed, and the resulting yellow solid is crystallized from EtOAc/hexane to give the pure product as a yellow solid. MS: m/z (EI+) 264.1.

1. temperatureAfter cooling to ambient temperature
2. customthe precipitate is removed by filtration
3. washrinsed with ethyl acetate
4. washThe filtrate is washed with 1 M aqueous citric acid, water, and brine
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. customThe solvent is removed
8. customthe resulting yellow solid is crystallized from EtOAc/hexane