反应详情

A mixture of compound 15 (2.5 g), intermediate 5 (1.65 g) and sodium carbonate (0.64 g) in methylisobutylketon (50 ml) was stirred and refluxed for 3 hours. The reaction mixture was washed and the separated organic layer was dried, filtered and the solvent was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 100/0 and 99.5/0.5). The pure fractions were collected and the solvent was evaporated, yielding 1.59 g (43%) of (±)-3,5-dimethylphenyl cis-4-[1-[3,5-bis(trifluoromethyl) benzoyl]-2-(phenylmethyl)-4-piperidinyl]-α-phenyl-1-piperazineacetate compound 43; mp. 88.1° C.).

1. temperaturerefluxed for 3 hours
2. washThe reaction mixture was washed
3. customthe separated organic layer was dried
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was purified over silica gel on a glass
7. filtrationfilter (eluent: CH2Cl2/CH3OH 100/0 and 99.5/0.5)
8. customThe pure fractions were collected
9. customthe solvent was evaporated