反应详情

A solution of 2-chloro-6-cyanopyridine (50 g) in THF (400 ml) is cooled to −5° C. and a solution of methylmagnesium iodide in diethyl ether (3 M, 200 ml) is added. After 1 h at 0° C. the ether is destilled off and the THF-mixture is heated to 60° C. for 1 h. The THF is evaporated and the residue is treated with ice water and acidified with 2 M hydrochloric acid. The water phase is extracted with dichloromethane and after drying and evaporation of the organic phase, the residue is purified by silica-gel flash chromatography. The title compound is obtained as an oil (11.2 g).

1. customThe THF is evaporated
2. additionthe residue is treated with ice water
3. extractionThe water phase is extracted with dichloromethane
4. customafter drying
5. customevaporation of the organic phase
6. customthe residue is purified by silica-gel flash chromatography