反应详情

A mixture of 10 g of 4-(2,3,4-trimethoxybenzylthio)piperidine and 6.62 g of cinnamyl bromide in 300 ml of CH3CN is heated under reflux for 15 hours in the presence of 4.64 g of potassium carbonate and 0.5 g of potassium iodide. The salt is then filtered off and the filtrate is evaporated under reduced pressure. The residue is taken up in CH2Cl2 --H2O and, after decantation, the ichloromethane phase is dried over Na2SO4 and evaporated under reduced pressure. The resulting residue (15 g) is purified by chromatography on 600 g of silica with a toluene-methanol (95-5) system, yielding 10 g of crude base, which is converted into the fumarate in an ethanol medium. 7 g of 4-(2,3,4-trimethoxybenzylthio)-1-cinnamylpiperidine fumarate are obtained in the form of white crystals which melt at 129° C.

1. temperatureis heated
2. filtrationThe salt is then filtered off
3. customthe filtrate is evaporated under reduced pressure
4. dry with materialH2O and, after decantation, the ichloromethane phase is dried over Na2SO4
5. customevaporated under reduced pressure
6. customThe resulting residue (15 g) is purified by chromatography on 600 g of silica with a toluene-methanol (95-5) system
7. customyielding 10 g of crude base, which