反应详情

温度

60 °C

To a 10 L jacketed vessel, fitted with a flange lid containing stirrer, thermometer and dropping funnel, was charged acetone (2.5 L) followed by 5-bromo-2,4-dihydroxybenzoic acid (100 g, 0.43 mol) and potassium carbonate (356 g, 2.58 mol). To the stirring mixture at ambient was added benzyl bromide (185 mL, 1.55 mol) at a rate of 20 ml/min. The mixture was heated at 60° C. for 18 h and then taken to 45° C. Water (1.5 L) was added and the mixture stirred for 30 min. The mixture was extracted with EtOAc (2×1 L) and the combined organic portions reduced in vacuo. To the residue was added Et2O (200 mL) and petroleum ether (1 L), the mixture stirred for 30 min and the solid formed collected by filtration and dried in vacuo to give the title compound (1 97.2 g) as a white solid.

1. customfitted with a flange lid
2. additioncontaining stirrer
3. customtaken to 45° C
4. extractionThe mixture was extracted with EtOAc (2×1 L)
5. additionTo the residue was added Et2O (200 mL) and petroleum ether (1 L)
6. stirringthe mixture stirred for 30 min
7. customthe solid formed
8. filtrationcollected by filtration
9. customdried in vacuo