反应详情

To a solution of 1-(2-methoxyphenyl)-4-[1-hydroxy-1-(2,4-dimethylphenyl)cyclohex-4-yl]piperazine in dichloromethane (anhydrous) at room temperature was added trifluoroacetic acid (8 equivalents). The solution was stirred overnight. Excess trifluoroacetic acid was removed under vacuo and the residue poured into sodium bicarbonate solution. The neutralised aqueous layer was extracted with dichloromethane, washed with salt solution, dried (MgSO4) and filtered. The solvent was removed and the residue purified by silica gel pressure column chromatography using hexane/ether (2/1) as eluant. The solid residue was recrystallised from ether to give the title compound which was converted to its dihydrochloride, m.p. 219° C. (dec.).

1. customExcess trifluoroacetic acid was removed under vacuo
2. additionthe residue poured into sodium bicarbonate solution
3. extractionThe neutralised aqueous layer was extracted with dichloromethane
4. washwashed with salt solution
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customThe solvent was removed
8. customthe residue purified by silica gel pressure column chromatography
9. customThe solid residue was recrystallised from ether