反应详情

A mixture of 14.8 parts of N-{4-(methoxymethyl)-1-[2-(4-nitrophenyl)ethyl]-4-piperidinyl}-N-phenylpropanamide and 200 parts of methanol is hydrogenated at normal pressure and at room temperature with 3 parts of Raney-nickel catalyst. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The oily residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The oily residue is triturated in petroleumether. The product is filtered off and crystallized from a small amount of 2,2'-oxybispropane. It is filtered off and dried, yielding 8.23 parts of N-{1-[2-(4-aminophenyl)ethyl]-4-(methoxymethyl)-4-piperidinyl}-N-phenylpropanamide; mp. 106.2° C.

1. filtrationthe catalyst is filtered off
2. customthe filtrate is evaporated
3. customThe oily residue is purified by column-chromatography over silica gel using
4. additiona mixture of trichloromethane and 5% of methanol as eluent
5. customThe pure fractions are collected
6. customthe eluent is evaporated
7. customThe oily residue is triturated in petroleumether
8. filtrationThe product is filtered off
9. customcrystallized from a small amount of 2,2'-oxybispropane
10. filtrationIt is filtered off
11. customdried