反应详情

温度

110 °C

A mixture of 4-bromo-2,5-difluoroaniline (5.0 g), ethyl crotonate (4.98 ml), palladium acetate (54.0 mg), tris(2-methylphenyl)phosphine (442 mg), and triethylamine (33.4 ml) was stirred at 110° C. in a nitrogen atmosphere for 48 hours. The reaction mixture was filtered through Celite, and the filtrate was concentrated. The obtained residue was 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 purified by column chromatography (5% ethyl acetate/n-hexane) to give Compound 10a (1.69 g, 29%) as a brown solid.

1. filtrationThe reaction mixture was filtered through Celite
2. concentrationthe filtrate was concentrated
3. customThe obtained residue was separated with ethyl acetate and water
4. washThe organic layer was washed with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off
7. customthe residue was purified by column chromatography (5% ethyl acetate/n-hexane)