反应详情

温度

110 °C

A mixture of 4-[2-(5-bromo-2-chloro-pyridin-4-yl)-1-hydroxy-ethyl]-piperidine-1-carboxylic acid tert-butyl ester (11.60 g), palladium acetate (500 mg), racemic 2-(di-tert-butylphosphino)-1,1′-binapthyl (1.00 g), and cesium carbonate (14.00 g) in toluene (150 mL) is heated in an oil bath at 110° C. under an argon atmosphere for 5 h. After cooling to room temperature ethyl acetate and water are added and the organic phase is separated, washed with brine, dried over MgSO4, and concentrated in vacuo. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 70:30→50:50) to give the title compound. LC (method 7): tR=1.44 min; Mass spectrum (ESI+): m/z=339 [M+H]+.

1. additionare added
2. customthe organic phase is separated
3. washwashed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 70:30→50:50)