Hydroxylamine → 2-Acetyl-4-(pyrid-2-yl)-pyrimidine oxime

HRID 933

Reaktionsgleichung

Reaktionsgleichung von HRID 933
[C:1]([C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][N:5]=1)(=O)[CH3:2].[NH2:16][OH:17].C([O-])(=O)C.[Na+]>C(O)C.O>[C:1](=[N:16][OH:17])([C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][N:5]=1)[CH3:2]

Komponenten

6

Edukt 3

HCID 787HydroxylamineHCID 517045Sodium AcetateHCID 196942132-Acetyl-4-(pyrid-2-yl)-pyrimidine

Produkt 1

HCID 1363959922-Acetyl-4-(pyrid-2-yl)-pyrimidine oximeAusbeute 91,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

A solution of 2-acetyl-4-(pyrid-2-yl)-pyrimidine (1.0 g), hydroxylamine (0.39 g) and sodium acetate (0.62 g) in a mixture of ethanol (10 ml) and water (2 ml) was heated to reflux for 1.5 hours. The reaction was then poured into water the precipitate filtered and washed with hexane to give 2-acetyl-4-(pyrid-2-yl)-pyrimidine oxime (0.98 g, 91% yield) as a white crystalline solid m.p. 196°-8° C.; 1H NMR: 2.50(3H,s); 7.42(1H,m); 7.88(1H,m); 8.30(1H,d); 8.59(1H,d); 8.74(1H,d); 8.90(1H,d); 10.85(1H,brs) ppm.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 1.5 hours
  3. filtrationfiltered
  4. washwashed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-25314cafe14044c4a971af24b93211f4
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05723473

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