反应详情

温度

83 °C

Pyridinium toluene-4-sulfonate (49 mg, 0.19 mmol) was added to a mixture of 4-fluoro-2-hydroxybenzamide (0.3 g, 1.93 mmol) in 2,2-dimethoxypropane (5 mL) and heated at 83° C. for 20 hours. The reaction mixture was reduced in vacuo and ethyl acetate (30 mL) added. The mixture was washed with 10% potassium carbonate solution (2×20 mL), brine (20 mL), dried (MgSO4), and reduced in vacuo to give a white solid. The material was chromatographed on silica, eluting with 40-70% ethyl acetate in isohexane, to give the desired compound as a white solid (0.26 g).

1. additionadded
2. washThe mixture was washed with 10% potassium carbonate solution (2×20 mL), brine (20 mL)
3. dry with materialdried (MgSO4)
4. customto give a white solid
5. customThe material was chromatographed on silica
6. washeluting with 40-70% ethyl acetate in isohexane