反应详情

温度

120 °C

Benzophenonimine (2.22 g) was added to a suspension of 4-(5-bromopyridin-2-yl)-1-(2-hydroxy-2-methylpropyl)piperidine-4-carbonitrile (3.95 g), palladium (II) acetate (328 mg), racemic-2-(di-tert-butylphosphino)-1,1′-binaphthyl (909 mg) and sodium tert-butoxide (1.68 g) in toluene (29 ml), and stirred at 120° C. for 2.5 hours. The reaction solution was left stand, a mixture of concentrated hydrochloric acid (2 ml) and water (6 ml) were added at 60-80° C. and stirred at room temperature. A saturated aqueous solution of sodium bicarbonate was added to the reaction solution and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified with basic silica gel column chromatography (n-hexane/ethyl acetate) to give the titled compound (2.6 g) as a pale yellow solid.

1. waitThe reaction solution was left stand
2. additionwere added at 60-80° C.
3. stirringstirred at room temperature
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified with basic silica gel column chromatography (n-hexane/ethyl acetate)