反应详情

A mixture of (±)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(phenylmethyl)-4-(1-piperazinyl)piperidine (0.0127 mol), chloroacetonitrile (0.013 mol) and sodium carbonate (0.013 mol) in methylisobutyl keton (100 ml) was stirred and refluxed. The mixture was cooled and water was added. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 100/0, 99.5/0.5 and 99/1). The pure fractions were collected and the solvent was evaporated, yielding 3.64 g (53%) of (±)-cis-1-[3,5-bis (trifluoromethyl)benzoyl]-4-[4-(cyanomethyl)-1-piperazinyl]-2-(phenylmethyl)piperidine (intermediate 6).

1. temperaturerefluxed
2. temperatureThe mixture was cooled
3. customThe organic layer was separated
4. customdried
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was purified over silica gel on a glass
8. filtrationfilter (eluent: CH2Cl2/CH3OH 100/0, 99.5/0.5 and 99/1)
9. customThe pure fractions were collected
10. customthe solvent was evaporated