反应详情

A mixture of compound 15 (0.005 mol) and 1,2-epoxyethylbenzene (0.006 mol) in methanol (50 ml) was stirred at RT for 1 hour. The mixture was stirred and refluxed for 3 hours. The solvent was evaporated and the residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 100/0, 99/1 and 98/2). The pure fractions were collected and the solvent was evaporated. The residue was purified by HPLC over silica gel (eluent: CH2Cl2/CH3OH 98/2 to 95/5). Two pure fractions were collected and their solvents were evaporated. Each residue was dried, yielding 0.7 g (23%) of (±)-cis-1-[3,5-bis(trifluoromethyl)benzoyl]-4-[4-(2-hydroxy-2-phenylethyl)-1piperazinyl]-2-(phenylmethyl)piperidine (compound 60) and 0.23 g (7%) of (±)-cis-1-[3,5-bis(trifluoromethyl)benzoyl]-4-[4-(2-hydroxy-2-phenylethyl)-1piperazinyl]-2-(phenylmethyl) piperidine (compound 61).

1. stirringThe mixture was stirred
2. temperaturerefluxed for 3 hours
3. customThe solvent was evaporated
4. customthe residue was purified over silica gel on a glass
5. filtrationfilter (eluent: CH2Cl2/CH3OH 100/0, 99/1 and 98/2)
6. customThe pure fractions were collected
7. customthe solvent was evaporated
8. customThe residue was purified by HPLC over silica gel (eluent: CH2Cl2/CH3OH 98/2 to 95/5)
9. customTwo pure fractions were collected
10. customtheir solvents were evaporated
11. customEach residue was dried