反应详情

A 3.7 g. portion of 3-(phenylaminomethyl)pyridine was dissolved in 20 ml. of dichloromethane, and to it was added 4.1 g. of potassium carbonate and 2.5 ml. of methanesulfonyl chloride. The mixture was stirred under reflux overnight, and was then diluted with 20 ml. of aqueous sodium bicarbonate and 20 ml. of dichloromethane. The organic phase was separated, washed with 20 ml. of water, dried over magnesium sulfate and evaporated under vacuum. The residue was triturated with diethyl ether and dried to give 4.9 g. of impure product. It was dissolved in 10 ml. of dichloromethane and 20 ml. of ethyl acetate and filtered. The filtrate was evaporated under vacuum, and the residue was triturated with petroleum ether, filtered and dried to obtain 4.4 g. of the desired product, m.p. 104°-105°.

1. temperatureunder reflux overnight
2. additionwas then diluted with 20 ml
3. customThe organic phase was separated
4. washwashed with 20 ml
5. dry with materialof water, dried over magnesium sulfate
6. customevaporated under vacuum
7. customThe residue was triturated with diethyl ether
8. customdried
9. customto give 4.9 g
10. dissolutionIt was dissolved in 10 ml
11. filtrationof ethyl acetate and filtered
12. customThe filtrate was evaporated under vacuum
13. customthe residue was triturated with petroleum ether
14. filtrationfiltered
15. customdried
16. customto obtain 4.4 g