反应详情

温度

112 °C

First, 0.93 g (6.36 mmol) of 3-phenyl-2-butenal and 0.99 g (5.91 mmol) of benzenesulfonyl cyanide were introduced to a 3-necked flask (25 ml volume) equipped with a thermometer, a magnetic stirrer, a Dean-Stark water type distilling receiver, and a condenser tube. Toluene (5 ml) as the solvent and butanol (0.5 ml) were added, and 0.14 g (0.59 mmol) of tributyl borate was added. Then the mixture was heated under reflux for 2 hours while agitating at an internal temperature of 112° C. in a nitrogen atmosphere, separating and removing water that was produced. After this solution was cooled to room temperature, the low-boiling components, such as solvent, etc., were removed under reduced pressure to give the desired, crude product. The crude product was purified by silica gel column chromatography (eluting solvent: ethyl acetate/hexane=1/4) to give 1.20 g of 2-benzenesulfonyl-4-phenylpyridine with the following properties as colorless crystals (purity of 99%, yield of 71% based on benzenesulfonyl cyanide).

1. customequipped with a thermometer, a magnetic stirrer
2. distillationa Dean-Stark water type distilling receiver, and a condenser tube
3. additionToluene (5 ml) as the solvent and butanol (0.5 ml) were added
4. temperatureThen the mixture was heated
5. temperatureunder reflux for 2 hours
6. customseparating
7. customremoving water that
8. customwas produced
9. temperatureAfter this solution was cooled to room temperature
10. customthe low-boiling components, such as solvent, etc., were removed under reduced pressure
11. customto give the
12. customThe crude product was purified by silica gel column chromatography (eluting solvent: ethyl acetate/hexane=1/4)