反应详情

温度

100 °C

A mixture of 270 mg of 4-benzyl-5-bromo-2-(4-hydroxypiperidino)pyridine, 130 mg of 3-ethynyl-3-quinuclidinol, 50 mg of tetrakis(triphenylphosphine)palladium(0), 2 mg of cuprous iodide, 0.35 ml of triethylamine and 2 ml of N,N-dimethylformamide was stirred at 100° C. for 3 hours in a nitrogen atmosphere. After cooling as it was, the reaction solution was extracted with ethyl acetate-aqueous dilute ammonia. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and evaporated. The residue was subjected to NH-silica gel column chromatography and eluted with 20-100% ethyl acetate/hexane and then with 5% methanol/ethyl acetate, to give 120 mg of the target compound.

1. temperatureAfter cooling as it
2. extractionthe reaction solution was extracted with ethyl acetate-aqueous dilute ammonia
3. washThe organic phase was washed with water and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customevaporated
6. washeluted with 20-100% ethyl acetate/hexane