反应详情

Heat at reflux for 8 hours, under a nitrogen atmosphere, a solution of 1.37 mmol of 6-hydroxy -2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin, 4.5 mmol of nicotinoyl chloride and 3.42 mmol of anhydrous pyridine in 25 cm3 of dichloroethane. After cooling, the reaction mixture is washed with a saturated aqueous solution of sodium hydrogen carbonate, dried over magnesium sulfate and then concentrated under reduced pressure. The crude product is then purified by chromatography on a silica column (eluant:petroleum ether/ethyl acetate, 70:30). 6-Nicotinoyloxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin is thereby obtained in a yield of 95%.

1. temperatureHeat
2. temperatureat reflux for 8 hours, under a nitrogen atmosphere
3. temperatureAfter cooling
4. washthe reaction mixture is washed with a saturated aqueous solution of sodium hydrogen carbonate
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe crude product is then purified by chromatography on a silica column (eluant:petroleum ether/ethyl acetate, 70:30)