反应详情

To a solution of 2-Bromo-5-hydroxy-benzoic acid methyl ester (80 g, 347 mmol) and K2CO3 (71.9 g, 520 mmol) in DMF (800 mL) was added BnBr (500 g, 416.2 mmol) at RT. The mixture was stirred at RT under N2 for 5 hr. The reaction mixture was diluted with H2O (500 mL) and extracted with ethyl acetate (100 mL*3). The organic phase was washed with saturated sodium bicarbonate solution 500 mL, dried over Na2SO4. After concentration, the crude product was purified by silica gel chromatography eluted with PE:EA=4:1 to give title product (100 g, 90% yield) as an off-white solid.

1. extractionextracted with ethyl acetate (100 mL*3)
2. washThe organic phase was washed with saturated sodium bicarbonate solution 500 mL
3. dry with materialdried over Na2SO4
4. concentrationAfter concentration
5. customthe crude product was purified by silica gel chromatography
6. washeluted with PE