반응 #56004

반응 방정식

hydrogen

1-(4-methoxyphenyl)piperazine dihydrochloride

1-butanal

sodium acetate

→

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

수율 81.0%

용매

methanol

반응 조건

후처리

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

실험 절차

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.

출처