تفاعل #2061027

معادلة التفاعل

N-{4-(methoxymethyl)-1-[2-(4-nitrophenyl)ethyl]-4-piperidinyl}-N-phenylpropanamide

hydrogen

→

N-{1-[2-(4-aminophenyl)ethyl]-4-(methoxymethyl)-4-piperidinyl}-N-phenylpropanamide

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe catalyst is filtered off
2. 2
   أخرىthe filtrate is evaporated
3. 3
   أخرىThe oily residue is purified by column-chromatography over silica gel using
4. 4
   workup.ADDITIONa mixture of trichloromethane and 5% of methanol as eluent
5. 5
   أخرىThe pure fractions are collected
6. 6
   أخرىthe eluent is evaporated
7. 7
   أخرىThe oily residue is triturated in petroleumether
8. 8
   ترشيحThe product is filtered off
9. 9
   أخرىcrystallized from a small amount of 2,2'-oxybispropane
10. 10
    ترشيحIt is filtered off
11. 11
    أخرىdried

الإجراء التجريبي

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.

المصدر