反应详情

A 2.3 g. portion of 3-(4-fluorophenylaminomethyl)pyridine was dissolved in 15 ml. of dichloromethane, and 2.1 g. of potassium carbonate and 1.2 ml. of methanesulfonyl chloride were added. The mixture was stirred under reflux for 2 days, and was then cooled and diluted with 20 ml. of aqueous sodium bicarbonate and 5 ml. of 2N sodium hydroxide. The organic phase was washed again with aqueous sodium bicarbonate, dried over magnesium sulfate and evaporated under vacuum. The residue was triturated with hot diethyl ether, and the solids were filtered and dried to obtain 2.6 g. of the desired product, m.p. 112°-113°.

1. temperatureunder reflux for 2 days
2. temperaturewas then cooled
3. additiondiluted with 20 ml
4. washThe organic phase was washed again with aqueous sodium bicarbonate
5. dry with materialdried over magnesium sulfate
6. customevaporated under vacuum
7. customThe residue was triturated with hot diethyl ether
8. filtrationthe solids were filtered
9. customdried
10. customto obtain 2.6 g