反应详情

温度

70 °C

(S)-N-(Pyrrolidin-3-yl)-1-adamantanecarboxamide (1.0 g) and 2-(4-cyanophenyl)ethyl p-toluenesulfonate (1.2 g) were dissolved in acetonitrile, and potassium carbonate was added thereto. The mixture was stirred under heating at 70° C. for 5 hours. After the completion of the reaction, the solvent was evaporated under reduced pressure. Ethyl acetate was added to the obtained residue and the mixture was washed with saturated brine. The solvent was evaporated under reduced pressure, and the obtained residue was subjected to silica gel column chromatography (chloroform:methanol=30:1). The obtained eluate was concentrated and IPE was added to the obtained residue. The precipitated crystals were collected by filtration to give (S)-N-(1-(2-(4-cyanophenyl)ethyl)pyrrolidin-3-yl)-1-adamantanecarboxamide (1.1 g), melting point 104-105° C.

1. customAfter the completion of the reaction
2. customthe solvent was evaporated under reduced pressure
3. additionEthyl acetate was added to the obtained residue
4. washthe mixture was washed with saturated brine
5. customThe solvent was evaporated under reduced pressure
6. concentrationThe obtained eluate was concentrated
7. additionIPE was added to the obtained residue
8. filtrationThe precipitated crystals were collected by filtration