Bis(2-pyridyl) ketone → Di-2-pyridinylmethanone oxime

HRID 963421

Reaktionsgleichung

Reaktionsgleichung von HRID 963421
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)=O.Cl.[NH2:16][OH:17]>N1C=CC=CC=1>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=[N:16][OH:17])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1

Komponenten

4

Edukt 2

HCID 88065Bis(2-pyridyl) ketoneHCID 443297Hydroxyamine hydrochloride

Produkt 1

HCID 73805Di-2-pyridinylmethanone oximeAusbeute 136,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2 g of di-2-pyridyl-ketone and 1.51 g of hydroxylamine-hydrochloride are added to 13 ml of pyridine and the mixture is held at reflux for 4 hrs. After concentration and cooling there are isolated 2.95 g of crude di-2-pyridyl ketone oxime (contaminated with salts). Addition of 1.18 g of ammonium acetate, 44 ml of dil. ammonia, 30 ml of water and 30 ml of ethanol yields a suspension which is treated portionwise with 4.5 g of zinc powder. The mixture is held at reflux for 4 hrs., cooled and suction filtered. The filtrate is concentrated and the residue is triturated with methanol. 2.54 g of crude C,C-dipyridin-2-yl-methylamine are isolated. Yield: 93%.

Aufarbeitung

  1. temperatureat reflux for 4 hrs
  2. concentrationAfter concentration
  3. temperaturecooling there

Quellen und Nachweise

ORD-Eintrag
ord-34628b93ec4e4430a53d5b08914c432a
Quelldatensatz
uspto-grants-1998_06
Patentnummer
US05763450

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