Ethylenediamine → N1-(pyridin-4-yl)ethane-1,2-diamine

HRID 614365

Reaktionsgleichung

Reaktionsgleichung von HRID 614365
Cl.Br[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.[CH2:9]([NH2:12])[CH2:10][NH2:11]>>[NH2:11][CH2:10][CH2:9][NH:12][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1

Komponenten

3

Edukt 2

HCID 3301EthylenediamineHCID 881004-Bromopyridinium chloride

Produkt 1

HCID 14834209N1-(pyridin-4-yl)ethane-1,2-diamine

Versuchsvorschrift

A mixture of 38.9 g of 4-bromo-pyridine-hydrochloride and 480 g of ethylenediamine is refluxed with stirring for 13 hours. The reaction mixture is thereafter concentrated under reduced pressure and the residue is treated with toluene and concentrated once more. The residue is made alkaline with a concentrated aqueous solution of sodium hydroxide and extracted with five 75 ml portions of methylene chloride. The combined extracts are dried over sodium sulphate and concentrated under reduced pressure. Recrystallisation of the residue from methylene chloride yields 4-(2-aminoethylamino)-pyridine as a light yellow crystalline substance with a melting point of 120°-121° C.

Aufarbeitung

  1. temperatureis refluxed
  2. concentrationThe reaction mixture is thereafter concentrated under reduced pressure
  3. additionthe residue is treated with toluene
  4. concentrationconcentrated once more
  5. extractionextracted with five 75 ml portions of methylene chloride
  6. dry with materialThe combined extracts are dried over sodium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customRecrystallisation of the residue from methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-5b5683f49b9c4128b6fd1fc128486bcb
Quelldatensatz
uspto-grants-1979_03
Patentnummer
US04144344

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