反应详情

To a solution of 1-bromo-3-fluorobenzyl bromide (1.75 kg, 6.52 mol) and 2-bromo-5-fluorophenol (730 mL, 16.56 mol, 1.01 eq) in N,N-dimethylformamide (14 L) at 0° C. add potassium carbonate (1.36 kg, 9.80 mol) in one portion and stir the resulting slurry cold for one hour and then at room temperature overnight. Transfer the reaction mixture to a 50 liter flask, add water (14 L) drop wise over 30 min and ice periodically to control the exotherm of the crystallization. Stir at room temperature for one hour, collect off-white solids by filtration, wash with water, and dry overnight at 50° C. to obtain the title compound (2.22 kg, 90%). 1H NMR (CDCl3) δ 7.51 (m, 2H), 7.30 (m, 1H), 7.14 (t, 1H), 6.89 (dd, 1H), 6.67 (m, 1H), 5.26 (d, 2H).

1. customat room temperature
2. customovernight
3. customthe exotherm of the crystallization
4. stirringStir at room temperature for one hour
5. customcollect off-white solids
6. filtrationby filtration
7. washwash with water
8. customdry overnight at 50° C.