تفاعل #56004

ord-75c12c2f42ce4758abaa9a2e21396e09

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04223036uspto-grants-1980_09