反应详情

温度

23 °C

A Grignard solution of 12.9 g (0.049 mol) of 4-chloro-2-fluoro-5-methoxyphenylmagnesium bromide in 60 ml of THF was added with stirring at 23-30° C. to a solution of 10 g (0.0392 mol) of 5-chloro-3-fluoro-2-phenylsulfinylpyridine in 150 ml of THF over a period of 10 min, and the mixture was stirred at 23° C. for another 4 h. The reaction mixture was concentrated under reduced pressure, taken up in methylene chloride and extracted in succession with 1 N hydrochloric acid, 1 N of aqueous sodium hydroxide solution and with water, and dried. The solution was filtered with suction through silica gel, concentrated, stirred with pentane, filtered off with suction and dried, affording 5.7 g (50.1% of theory) of the title compound of mp. 120-122° C.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionextracted in succession with 1 N hydrochloric acid, 1 N of aqueous sodium hydroxide solution and with water
3. customdried
4. filtrationThe solution was filtered with suction through silica gel
5. concentrationconcentrated
6. stirringstirred with pentane
7. filtrationfiltered off with suction
8. customdried