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

HRID 1156287

反応式

HRID 1156287 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 205193341-Butyl-4-(4-methoxyphenyl)piperazine dihydrochloride収率 81%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

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. Upon 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.

後処理

  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. additionUpon 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

出典と根拠

ORDレコード
ord-b206d30cabf54b479e251fd609922b08
出典データセット
uspto-grants-1982_06
特許番号
US04335125

関連ノート

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