反应详情

Titanium(IV)isopropoxide (16.5 g) was added to a mixture of intermediate 3 (21.5 g) and 1-(phenylmethyl)piperazine (8.81 g) in DCM (35 ml). The mixture was stirred for 3 hours at RT. Sodium cyanoborohydride (2.85 g) and ethanol (70 ml) were added and the resulting reaction mixture was stirred overnight at RT. Water (5 ml) and DCM were added. The biphasic mixture was filtered over dicalite, and the filter residue was washed with DCM. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was crystallized from CH3CN and the precipitate was filtered off and dried, yielding 7.93 g (26.9%) of (±)-cis-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(phenylmethyl)-4-[4-(phenylmethyl)-1-piperazinyl]piperidine (compound 16; mp. 143.8° C.).

1. customthe resulting reaction mixture
2. stirringwas stirred overnight at RT
3. filtrationThe biphasic mixture was filtered over dicalite
4. washthe filter residue was washed with DCM
5. customThe organic layer was separated
6. customdried
7. filtrationfiltered
8. customthe solvent was evaporated
9. customThe residue was crystallized from CH3CN
10. filtrationthe precipitate was filtered off
11. customdried