反应详情

A 3-l. three-necked flask, equipped with mechanical stirrer, reflux condenser and thermometer was charged under nitrogen with 155 g of 3-(2-methyl-1,3-dioxolan-2-yl)pyridine and 1.2 l of toluene. 272 g of methyl iodide was added. The mixture was stirred and heated at 53° (internal temp.) for 32 hours and then let stand at room temperature overnight. The precipitate was collected by filtration, washed with 500 ml of toluene, 500 ml of hexane and dried (r.t., 0.1 mm, const. weight) to yield 286.2 g (99.3%) of 1-methyl-3-(2-methyl-1,3-dioxolan-2-yl)pyridinium iodide as light yellow crystals, m.p. 185.5°-187° (sinters at 167°).

1. customthree-necked flask, equipped with mechanical stirrer
2. temperaturereflux condenser
3. temperatureheated at 53° (internal temp.) for 32 hours
4. filtrationThe precipitate was collected by filtration
5. washwashed with 500 ml of toluene, 500 ml of hexane
6. customdried (r.t., 0.1 mm, const. weight)