反应详情

To a stirred mixture of the (6-chloropyridin-3-yl)acetonitrile (8.00 g, 0.0524 mol), benzyltriethylammonium chloride (0.8 g, 0.004 mol), and 1-bromo-2-chloro-ethane (8.69 mL, 0.105 mol) was added dropwise sodium hydroxide, 50% aqueous solution (16.1 mL, 0.419 mol) at 50° C. After stirring for 2 h, the reaction mixture was diluted with water and the resulting layers were separated. The aqueous layer was extracted with dichloromethane. The combined organic layers were washed with 1N HCl and brine successively, dried with magnesium sulfate, filtered, and concentrated in-vacuo. The crude product was purified by combiflash to obtain 2.5 g of pure product as a white solid.

1. customthe resulting layers were separated
2. extractionThe aqueous layer was extracted with dichloromethane
3. washThe combined organic layers were washed with 1N HCl and brine successively
4. dry with materialdried with magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in-vacuo
7. customThe crude product was purified by combiflash