反应详情

温度

100 °C

2-Amino-5-bromopyridine (15 g) was dissolved in a mixed solvent of N,N-dimethylformamide (hereinafter referred to as “DMF”; 60 ml) and N,N-diisopropylethylamine (60 ml). Ethyl acrylate (12 ml), palladium acetate (980 mg), and tris(2-methylphenyl)phosphine (10.5 g) were added thereto in a nitrogen atmosphere, and the mixture was stirred at 100° C. for 12 hours. The reaction mixture was filtered through Celite and separated with ethyl acetate and water. The organic layer was washed with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was crystallized with N-hexane to obtain Compound 1a (15.5 g, 89%) as a yellow solid.

1. filtrationThe reaction mixture was filtered through Celite
2. customseparated with ethyl acetate and water
3. washThe organic layer was washed with a saturated sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was distilled off
6. customthe residue was crystallized with N-hexane