Potassium Iodide → N,N-dimethyl N'-[2-(3-pyridyl)ethyl]ethanediamine

HRID 129810

Reaktionsgleichung

Reaktionsgleichung von HRID 129810
Cl.Cl[CH2:3][CH2:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][CH:10]=1.[CH3:11][N:12]([CH3:16])[CH:13]([NH2:15])[CH3:14].C(=O)(O)[O-].[Na+].[I-].[K+]>C(O)C>[CH3:11][N:12]([CH3:16])[CH:13]([NH:15][CH2:3][CH2:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][CH:10]=1)[CH3:14]

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 199465Pyridine, 3-(2-chloroethyl)-, hydrochlorideHCID 516892Sodium BicarbonateHCID 18943179N~1~,N~1~-Dimethylethane-1,1-diamine

Produkt 1

HCID 18788472N,N-dimethyl N'-[2-(3-pyridyl)ethyl]ethanediamineAusbeute 56,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

11 g of 3-(2-chloroethyl)pyridine hydrochloride, 16.3 g of N,N-dimethylethane diamine, 18.5 g of sodium bicarbonate and 13 g of potassium iodide are heated in 150 ml of ethanol for about 30 hours at about 60° C. The solvent is evaporated and the residue is taken up in 100 ml of water before an aqueous solution of 10N NaOH is added to give pH 8; the aqueous phase is then extracted 3 times with 80 ml of ethyl acetate. The pooled organic phases are dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residual oil is distilled to give 6.7 g of the expected product.

Aufarbeitung

  1. customThe solvent is evaporated
  2. additionis added
  3. customto give pH 8
  4. extractionthe aqueous phase is then extracted 3 times with 80 ml of ethyl acetate
  5. dry with materialThe pooled organic phases are dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. distillationThe residual oil is distilled

Quellen und Nachweise

ORD-Eintrag
ord-90c7c5d20a114624b6aae3318d1b3f37
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05470855

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