反应详情

温度

90 °C

To 4-chlorophenol (2.0 g, 15.5 mmol) and chloromethylphthalamide (2.62 g, 13.4 mmol) was added zinc chloride (3 mL, 0.5 M in tetrahydrofuran, 1.5 mmol). The reaction was stirred at 90° C. for 48 hours. After cooling the reaction was diluted with methanol (15 mL) and brought to reflux. After 30 minutes the hot suspension was filtered through a medium glass frit and concentrated to an off-white solid. Methanol (50 mL) was again added and the reaction brought to reflux. After 3 hours the hot suspension was filtered through a medium glass frit and concentrated to an off-white solid. The crude product was purified via chromatography on silica gel to give the title compound (3.86 g).

1. temperatureAfter cooling the reaction
2. temperatureto reflux
3. filtrationAfter 30 minutes the hot suspension was filtered through a medium glass frit
4. concentrationconcentrated to an off-white solid
5. additionMethanol (50 mL) was again added
6. temperatureto reflux
7. filtrationAfter 3 hours the hot suspension was filtered through a medium glass frit
8. concentrationconcentrated to an off-white solid
9. customThe crude product was purified via chromatography on silica gel