Hydrochloric Acid → 1-(3,3-Diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride

HRID 1076784

Reaktionsgleichung

Reaktionsgleichung von HRID 1076784
[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]=[C:30]([O:34][CH3:35])[C:31]=1[O:32][CH3:33])[CH2:27][Cl:28].[ClH:36]>C1(C)C=CC=CC=1>[ClH:28].[ClH:36].[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]=[C:30]([O:34][CH3:35])[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 774485-(Chloromethyl)-1,2,3-trimethoxybenzeneHCID 10356330N-3,3-Diphenylpropylpiperazine

Produkt 1

HCID 215378221-(3,3-Diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochlorideAusbeute 80,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

N-3,3-Diphenylpropylpiperazine in the amount of 2.8 g (0.01 mole) and 2.2 g (0.01 mole) of 3,4,5-trimethoxybenzyl chloride were dissolved in 20 ml of toluene, and heated at the refluxing temperature for 4.5 hours. After the reaction liquid was left to cool, dry hydrogen chloride gas was passed through the reaction liquid while cooling the liquid to precipitate crystals of 1-(3,3-diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride, which were recrystallized from an ethanol and ether mixed solvent to obtain 4.3 g of pure crystals (80.6% yield) with a melting point of 178°C.

Aufarbeitung

  1. temperatureheated at the refluxing temperature for 4.5 hours
  2. customAfter the reaction liquid
  3. waitwas left
  4. temperatureto cool
  5. temperaturewhile cooling the liquid
  6. customto precipitate crystals of 1-(3,3-diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride, which
  7. customwere recrystallized from an ethanol and ether mixed solvent

Quellen und Nachweise

ORD-Eintrag
ord-61a6bde97eb94f88a3a73efddef856ca
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03957790

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