反应详情

A mixture of 0.54 g (1.2 mmols) of 2-ethoxy-4-[N-{1-(2-piperidino-phenyl)-1-butyl}-aminocarbonylmethyl]-benzyl chloride (melting point 114°-115° C., prepared from 2-ethoxy-4-[N-{1-(2-piperidino-phenyl)-1-butyl}-aminocarbonylmethyl-benzyl alcohol and thionyl chloride in chloroform) and 10 ml of absolute dioxane was hydrogenated for 3 hours at 20° C. and a pressure of 5 bar hydrogen. The reaction mixture was then evaporated in vacuo, and the residue was taken up in a mixture of ethyl acetate and aqueous sodium carbonate. The organic phase was dried, filtered and evaporated in vacuo. The evaporation residue was purified by column chromatography on silica gel (chloroform/acetone=19/1).

1. customThe reaction mixture was then evaporated in vacuo
2. additionthe residue was taken up in a mixture of ethyl acetate and aqueous sodium carbonate
3. customThe organic phase was dried
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe evaporation residue was purified by column chromatography on silica gel (chloroform/acetone=19/1)