反応 #56004

反応方程式

hydrogen

1-(4-methoxyphenyl)piperazine dihydrochloride

1-butanal

sodium acetate

→

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

収率 81.0%

溶媒

methanol

反応条件

後処理

1. 1
   ろ過the catalyst is filtered off
2. 2
   その他the filtrate is evaporated
3. 3
   workup.ADDITIONWater is added to the residue
4. 4
   その他the product is precipitated
5. 5
   ろ過It is filtered off
6. 6
   洗浄washed with water
7. 7
   workup.ADDITIONUnder the addition of 2,2'-oxybispropane
8. 8
   その他the salt is precipitated
9. 9
   ろ過It is filtered off
10. 10
    その他crystallized from a mixture of ethanol and 2,2'-oxybispropane

実験手順

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.

出典