反应详情

A solution of DMF (100 mL), 5-bromo-2,3-difluorophenol (10 g, 47.85 mol), and K2CO3 (7.27 g, 52.63 mol) and benzyl bromide (9 g, 52.63 mol) were combined at 0° C. under N2. The solution was allowed to warm to rt and stirred overnight. H2O, Et3N (2 eq) and EtOAc (5000 mL) were added and the organic layer separated. The aqueous layer was washed with EtOAc (2×) and the combined organic fractions were washed with 1M HCl (2×), sat. aq. NaHCO3 (2×), dried, and concentrated. The crude product was purified by Biotage (gradient 100% hexanes-60% EtOAc/hexanes) to afford 10.08 g of product as an oil.

1. customwere combined at 0° C. under N2
2. customthe organic layer separated
3. washThe aqueous layer was washed with EtOAc (2×)
4. washthe combined organic fractions were washed with 1M HCl (2×), sat. aq. NaHCO3 (2×)
5. customdried
6. concentrationconcentrated
7. customThe crude product was purified by Biotage (gradient 100% hexanes-60% EtOAc/hexanes)