Hydrochloric Acid → 1-(3,3-Diphenylpropyl)-4(3,4-dimethoxybenzyl)piperazine dihydrochloride

HRID 1076786Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076786
[C:1]1([CH:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:22][O:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][C:31]=1[O:32][CH3:33])[CH2:27][Cl:28].[ClH:34]>C(C(C)=O)C>[ClH:28].[ClH:34].[C:16]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([CH2:27][C:26]3[CH:29]=[CH:30][C:31]([O:32][CH3:33])=[C:24]([O:23][CH3:22])[CH:25]=3)[CH2:14][CH2:15]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 81740Veratryl chlorideHCID 10356330N-3,3-Diphenylpropylpiperazine

Produkt 1

HCID 215378181-(3,3-Diphenylpropyl)-4(3,4-dimethoxybenzyl)piperazine dihydrochlorideAusbeute 87,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

N-3,3-Diphenylpropylpiperazine in the amount of 2.8 g (0.01 mole) and 1.87 g (0.01 mole) of 3,4-dimethoxybenzyl chloride were dissolved in 20 ml of methyl ethyl ketone, and the resulting solution was heated at the refluxing temperature for 7.5 hours. After the reaction liquid was left to cool, dry hydrogen chloride gas was passed through the liquid while cooling the liquid to precipitate 1-(3,3-diphenylpropyl)-4-(3,4-dimethoxybenzyl)piperazine dihydrochloride. The crystals of this salt were recrystallized from an ethanol and ether mixed solvent to obtain 4.4 g (87.4% yield) of pure crystals with a melting point of 184°C.

Aufarbeitung

  1. temperaturethe resulting solution was heated at the refluxing temperature for 7.5 hours
  2. customAfter the reaction liquid
  3. waitwas left
  4. temperatureto cool
  5. temperaturewhile cooling the liquid
  6. customto precipitate 1-(3,3-diphenylpropyl)-4-(3,4-dimethoxybenzyl)piperazine dihydrochloride
  7. customThe crystals of this salt were recrystallized from an ethanol and ether mixed solvent

Quellen und Nachweise

ORD-Eintrag
ord-4c441f7d0045495d8deef7053b50f7a1
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03957790

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