Reacción #56004

Ecuación de reacción

hydrogen

1-(4-methoxyphenyl)piperazine dihydrochloride

1-butanal

sodium acetate

→

1-butyl-4-(4-methoxyphenyl)piperazine dihydrochloride

Rendimiento 81.0%

Disolventes

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   Filtraciónthe catalyst is filtered off
2. 2
   Otrothe filtrate is evaporated
3. 3
   workup.ADDITIONWater is added to the residue
4. 4
   Otrothe product is precipitated
5. 5
   FiltraciónIt is filtered off
6. 6
   Lavadowashed with water
7. 7
   workup.ADDITIONUnder the addition of 2,2'-oxybispropane
8. 8
   Otrothe salt is precipitated
9. 9
   FiltraciónIt is filtered off
10. 10
    Otrocrystallized from a mixture of ethanol and 2,2'-oxybispropane

Procedimiento

A mixture of 13.2 parts of 1-(4-methoxyphenyl)piperazine dihydrochloride, 5.1 parts of 1-butanal, 9 parts of sodium acetate and 80 parts of methanol is hydrogenated at normal pressure and at room temperature with 1 part of palladium-on-charcoal catalyst. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. Water is added to the residue and the product is precipitated. It is filtered off, washed with water and converted into the hydrochloride salt in ethanol and 2-propanol. Under the addition of 2,2'-oxybispropane, the salt is precipitated. It is filtered off and crystallized from a mixture of ethanol and 2,2'-oxybispropane, yielding 13.1 parts (81%) of 1-butyl-4-(4-methoxyphenyl)piperazine dihydrochloride; mp. 214.2° C.

Fuente