反应详情

To a mixture of ethyl 4-(piperazinyl)benzoate (2.00 g) and 4-methylenecyclohexan-1-one (0.98 g) in a mixture of methanol (40 ml) and acetic acid (1.47 ml) was portionwise added sodium cyanoborohydride (644 mg) with stirring under ice-cooling and the mixture was stirred at ambient temperature overnight. To the reaction mixture was added water (200 ml) and the mixture was adjusted to pH 8-9 with saturated aqueous sodium hydrogen carbonate. The resulting precipitates were collected and chromatographed on silica gel (200 ml) 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-[4-(4-methylenecyclohexyl)-1-piperazinyl]benzoate (1.39 g).

1. temperaturecooling
2. stirringthe mixture was stirred at ambient temperature overnight
3. customThe resulting precipitates
4. customwere collected
5. customchromatographed on silica gel (200 ml)
6. washeluting with a mixture of n-hexane and ethyl acetate (2:1 v/v)
7. additionThe fractions containing the desired compound
8. customwere collected
9. customevaporated under reduced pressure