反应详情

A mixture of 3 parts of cis-4-amino-5-chloro-N[1-(2-cyanoethyl)-3-methoxy-4-piperidinyl]-2-methoxybenzamide and 200 parts of methanol, saturated with ammonia was hydrogenated at normal pressure and at 20° C. with 2 parts of Raney-nickel catalyst. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was dissolved in trichloromethane. The solution was washed with water, dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried in vacuo at 60° C., yielding 0.4 parts (13%) of cis-4-amino-N-[1-(3-aminopropyl)-3-methoxy-4piperidinyl]-5-chloro-2-methoxybenzamide; mp. 174.8 (interm. 3).

1. filtrationthe catalyst was filtered off
2. customthe filtrate was evaporated
3. dissolutionThe residue was dissolved in trichloromethane
4. washThe solution was washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue was crystallized from acetonitrile
9. filtrationThe product was filtered off
10. customdried in vacuo at 60° C.