反应详情

Thionyl chloride (9.62 g, 81 mmol) was added to a solution of 3-fluoro-4-methylbenzoic acid (5.0 g, 32.4 mmol) in toluene (50 ml). The mixture was stirred at room temperature for 1.5 h and heated at reflux for 3 h. The sol-vent was removed in vacuo and the residue was taken up in methanol (30 ml) and CH2Cl2 (30 ml) and stirred for 18 h. The mixture was evaporated in vacuo and the residue was taken up in EtOAc (50 ml), washed with saturated NaHCO3 solution (3×75 ml), dried and evaporated in vacuo to yield the title compound (4.5 g, 83%).

1. temperatureheated
2. temperatureat reflux for 3 h
3. customThe sol-vent was removed in vacuo
4. stirringCH2Cl2 (30 ml) and stirred for 18 h
5. customThe mixture was evaporated in vacuo
6. washwashed with saturated NaHCO3 solution (3×75 ml)
7. customdried
8. customevaporated in vacuo