反应详情

温度

100 °C

3,5-Dihydroxybenzyl alcohol (5.0 g, 40 mmol), 2-chloro-5-trifluoromethyl-pyridine (7.13 g, 39.2 mmol) and potassium carbonate (6.16 g, 44.6 mmol) were suspended in dimethylformamide (100 mL) and heated to 100° C. After stirring for 16 h, the reaction was cooled to room temperature and partitioned between water (500 mL) and ethyl acetate. The organic layer was separated and the aqueous was extracted again with ethyl acetate. The combined organic layer was dried over sodium sulfate, filtered and concentrated. The residue was purified by silica gel chromatography (10-75%, EtOAc:heptane) to afford the title compound (2.32 g, 20% yield) as a thick oil.

1. temperaturethe reaction was cooled to room temperature
2. custompartitioned between water (500 mL) and ethyl acetate
3. customThe organic layer was separated
4. extractionthe aqueous was extracted again with ethyl acetate
5. dry with materialThe combined organic layer was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica gel chromatography (10-75%, EtOAc:heptane)