反应详情

A 8.9 g. portion of 3-(2,4-difluorophenylaminomethyl)pyridine was dissolved in 30 ml. of dichloromethane, and to it was added 6.9 g. of potassium carbonate and 3.9 ml. of methanesulfonyl chloride. The mixture was stirred at ambient temperature for several days, and then was heated and stirred at the reflux temperature overnight. It was then cooled, extracted with aqueous sodium bicarbonate, dried over magnesium sulfate and evaporated to a small volume. The residue was chromatographed over silica gel, eluting first with dichloromethane and then with 9:1 dichloromethane:ethyl acetate. The product-containing fractions were combined and evaporated to obtain impure product, which was triturated with diethyl ether and dried to obtain 5.6 g. of the desired product, m.p. 132°-135°.

1. temperaturewas heated
2. stirringstirred at the reflux temperature overnight
3. temperatureIt was then cooled
4. extractionextracted with aqueous sodium bicarbonate
5. dry with materialdried over magnesium sulfate
6. customevaporated to a small volume
7. customThe residue was chromatographed over silica gel
8. washeluting first with dichloromethane
9. customevaporated
10. customto obtain impure product, which
11. customwas triturated with diethyl ether
12. customdried
13. customto obtain 5.6 g