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HCID 18784149, Verbindung → HCID 18784192, Verbindung

HRID 1108759
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1108759
C([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=2)[CH2:10]1)C1C=CC=CC=1.[ClH:25].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:25].[CH3:24][O:23][C:17]1[CH:16]=[C:15]([CH:11]2[CH2:12][CH2:13][CH2:14][CH:9]([NH2:8])[CH2:10]2)[CH:20]=[CH:19][C:18]=1[O:21][CH3:22]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 18784149HCID 18784149, VerbindungHCID 21866389Hydrogen chloride-ethyl acetate

Produkt 1

HCID 18784192HCID 18784192, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

N-Benzyl-N-[3-(3,4-dimethoxyphenyl)cyclohexyl]amine (3.16 g) was dissolved in ethyl acetate, 4 N HCl-ethyl acetate solution was added, and the mixture was stirred at room temperature for 30 minutes. After concentrating the solvent under reduced pressure, it was dissolved in acetic acid (100 ml), and 10% palladium-carbon (640 mg) was added thereto. After substituting the reaction vessel with hydrogen gas, hydrogen addition was effected for 3 hours at normal pressure, at 80° C. After the reaction, the catalyst was filtered off and the solvent was distilled off under reduced pressure to produce crude crystals which were then washed with diethyl ether to give 2.80 g of 3-(3,4-dimethoxyphenyl)cyclohexylamine hydrochloride (quantitative yield).

Aufarbeitung

  1. concentrationAfter concentrating the solvent under reduced pressure, it
  2. dissolutionwas dissolved in acetic acid (100 ml)
  3. addition10% palladium-carbon (640 mg) was added
  4. additionwith hydrogen gas, hydrogen addition
  5. waitwas effected for 3 hours at normal pressure, at 80° C
  6. customAfter the reaction
  7. filtrationthe catalyst was filtered off
  8. distillationthe solvent was distilled off under reduced pressure
  9. customto produce crude crystals which
  10. washwere then washed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-1d5bbbffbe2544ab8687a4c74f8464fb
Quelldatensatz
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06069176

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