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Hydrochloric Acid → N-Methyl-N-[2-(3,4-dimethoxyphenyl)ethyl]-2-methyl-1,3-propanediamine

HRID 1769660
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1769660
[CH3:1][N:2]([CH2:15][CH:16]([CH3:19])[C:17]#[N:18])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=1.Cl>C(O)C.[Pt]=O>[CH3:1][N:2]([CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=1)[CH2:15][CH:16]([CH3:19])[CH2:17][NH2:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 199703153-[N-methyl-N-(2-(3,4-dimethoxyphenyl)ethyl)amino]-2-methylpropionitrile

Produkt 1

HCID 15045284N-Methyl-N-[2-(3,4-dimethoxyphenyl)ethyl]-2-methyl-1,3-propanediamineAusbeute 92,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 82844Platinum oxide (PtO)KatalysatorHCID 702Ethanol
Lösungsmittel

Versuchsvorschrift

2.1 g of the above nitrile and 0.2 ml of concentrated hydrochloric acid were dissolved in 30 ml of ethanol, followed by the addition of 0.2 g of platinum oxide to carry out hydrogenation under a hydrogen pressure of 2.1 kg/cm2. The reaction mixture was filtered to remove the catalyst. The filtrate was distilled under a reduced pressure to remove the ethanol. The residue was made alkaline with a dilute solution of caustic soda. The aqueous layer was extracted with dichloromethane. The extract was washed with water, dried over magnesium sulfate and distilled under a reduced pressure to obtain 1.98 g of the title compound as a pale yellow oil (yield: 38%).

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. customto remove the catalyst
  3. distillationThe filtrate was distilled under a reduced pressure
  4. customto remove the ethanol
  5. extractionThe aqueous layer was extracted with dichloromethane
  6. washThe extract was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled under a reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e265f410f1c1482cb453ef1c730b44b9
Quelldatensatz
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05382595

Notizen zur Reaktion

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