反应详情

温度

100 °C

A mixture of 4-nitro-3-(tetrahydro-2H-pyran-4-yloxy)phenol (23.0 g), 2-bromo-5-(methylsulfonyl)pyridine (22.7 g), cesium carbonate (62.6 g), and N,N-dimethylformamide (200 mL) was stirred at 100° C. for 1.5 hr. The reaction solution was concentrated under reduced pressure, water was added to the residue, and the mixture was extracted with ethyl acetate-tetrahydrofuran. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The obtained solid was washed with diethyl ether-hexane to give the title compound (30.0 g, yield 81%) as a brown solid.

1. concentrationThe reaction solution was concentrated under reduced pressure, water
2. additionwas added to the residue
3. extractionthe mixture was extracted with ethyl acetate-tetrahydrofuran
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. washThe obtained solid was washed with diethyl ether-hexane