反应详情

温度

190 °C

To a 500 mL round bottom flask was added 2-(3-methoxyphenyl)pyridine (21.3 g, 115 mmol) and pyridine hydrochloride (107.5 g, 930 mmol). The reaction mixture was heated to 190° C. for 8 hours under nitrogen. The reaction mixture was cooled slightly and water was added. The mixture was stirred overnight. The pH of the solution was adjusted to 7 with 10% sodium hydroxide solution, extracted three times with dichloromethane. The organic layers were washed with 10% LiCl solution, brine, dried over magnesium sulfate, filtered, and evaporated. The residue was distilled on a Kugelrohr to remove the remaining pyridine (18 g, 91%).

1. temperatureThe reaction mixture was cooled slightly
2. extractionextracted three times with dichloromethane
3. washThe organic layers were washed with 10% LiCl solution, brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customevaporated
7. distillationThe residue was distilled on a Kugelrohr
8. customto remove the remaining pyridine (18 g, 91%)