反应详情

温度

170 °C

In 70 ml of sulfolane were mixed 10.5 g of 2,5-bis(ethylsulfonyl)pyridine, 15.8 g of 2,4,5-trichlorophenol and 11.06 g of potassium carbonate. The mixture was warmed gradually to 170° C. and maintained at that temperature for 2 hrs. The reaction mixture was cooled and then poured into 300 g of ice containing 4 g of sodium hydroxide. The aqueous solution was extracted with ether. The organic layer was washed with water, dried over MgSO4 and concentrated. The product was purified using a Water's Prep LC 500 instrument with 10% ethyl acetate/90% hexane as eluent. Recrystallization from diethyl ether gave 2.8 g, (19% yield), of purified 5-(ethylsulfonyl)-2-(2,4,5-trichlorophenoxy)pyridine, m.p. 120°-122° C.

1. temperaturemaintained at that temperature for 2 hrs
2. temperatureThe reaction mixture was cooled
3. extractionThe aqueous solution was extracted with ether
4. washThe organic layer was washed with water
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe product was purified
8. customRecrystallization from diethyl ether