反应详情

A mixture of 0.50 g of 2-chloro-6-(1-chloromethylvinyl) pyridine, 0.88 g of potassium iodide, 5 ml of acetone and 0.5 ml of N,N-dimethylformamide was stirred at 50° to 60° C. for 5 hours. After the reaction mixture was cooled to room temperature, water was added thereto to extract the mixture with ethyl acetate. The extract was subsequently washed with an aqueous solution of 10% sodium thiosulfate, water, saturated saline solution in that order, and dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluted with dichloromethane) to obtain 0.45 g of the objective compound.

1. extractionto extract the mixture with ethyl acetate
2. washThe extract was subsequently washed with an aqueous solution of 10% sodium thiosulfate, water, saturated saline solution in that order
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationAfter distilling off the solvent
5. customthe residue was purified by silica gel column chromatography (eluted with dichloromethane)