反应详情

温度

140 °C

A mixture of cis-1-(4-methylcyclohexyl)piperazine (29.6 g), ethyl 4-fluorobenzoate (41.0 g) and potassium carbonate (67.3 g) in DMSO (300 ml) was stirred at 140° C. for 9 hours. The reaction mixture was poured into water (1.2 l) and extracted twice with ethyl acetate (400 ml). The extracts were collected, washed with saturated aqueous sodium chloride, dried over magnesium sulfate and evaporated in vacuo. The resulting residue was chromatographed on silica gel (1 l) eluting with a mixture of n-hexane and ethyl acetate (2:1 v/v). The fractions containing the desired compound were collected and evaporated under reduced pressure to give ethyl 4-[cis-4-(4-methylcyclohexyl)-1-piperazinyl]benzoate (37.64 g).

1. extractionextracted twice with ethyl acetate (400 ml)
2. customThe extracts were collected
3. washwashed with saturated aqueous sodium chloride
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe resulting residue was chromatographed on silica gel (1 l)
7. washeluting with a mixture of n-hexane and ethyl acetate (2:1 v/v)
8. additionThe fractions containing the desired compound
9. customwere collected
10. customevaporated under reduced pressure