Butanal → 1-Butyl-4-(4-methoxyphenyl)piperazine dihydrochloride

HRID 27726

반응식

HRID 27726 반응식
[ClH:1].Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.[CH:17](=O)[CH2:18][CH2:19][CH3:20].C([O-])(=O)C.[Na+].[H][H]>[Pd].CO>[ClH:1].[ClH:1].[CH2:17]([N:14]1[CH2:15][CH2:16][N:11]([C:8]2[CH:7]=[CH:6][C:5]([O:4][CH3:3])=[CH:10][CH:9]=2)[CH2:12][CH2:13]1)[CH2:18][CH2:19][CH3:20]

참가 물질

7

반응물 4

HCID 261ButanalHCID 517045Sodium AcetateHCID 27237001-(4-Methoxyphenyl)-piperazine, dihydrochlorideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 205193341-Butyl-4-(4-methoxyphenyl)piperazine dihydrochloride수율 81%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

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.

후처리

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. additionWater is added to the residue
  4. customthe product is precipitated
  5. filtrationIt is filtered off
  6. washwashed with water
  7. additionUnder the addition of 2,2'-oxybispropane
  8. customthe salt is precipitated
  9. filtrationIt is filtered off
  10. customcrystallized from a mixture of ethanol and 2,2'-oxybispropane

출처 및 근거

ORD 기록
ord-75c12c2f42ce4758abaa9a2e21396e09
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04223036

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