Oxalic Acid → 5-Trifluoromethyl-quinazoline-2,4-diamine

HRID 655621Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 655621
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8].[C:9](O)(=[O:13])[C:10](O)=[O:11]>Cl>[NH:8]1[C:10](=[O:11])[C:9](=[O:13])[NH:1][C:2]2[CH:3]=[N:4][CH:5]=[CH:6][C:7]1=2

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 59183,4-Diaminopyridine

Produkt 1

HCID 107970835-Trifluoromethyl-quinazoline-2,4-diamineAusbeute 81,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

To a suspension of 3,4-diaminopyridine (10 g, 0.068 mol) in 4N aqueous HCl (100 ml) is added oxalic acid (10.4 g, 0.082 mol) and the reaction mixture is refluxed for 20 h. The reaction mixture is cooled down and the solid precipitated is filtered, washed with water then dried under vacuum to afford 9 g (80%) of the title compound as a solid. HPLC (max plot) 98%. LC/MS: (ES+): 164.3.

Aufarbeitung

  1. temperaturethe reaction mixture is refluxed for 20 h
  2. temperatureThe reaction mixture is cooled down
  3. customthe solid precipitated
  4. filtrationis filtered
  5. washwashed with water
  6. customthen dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-60df395042a8448483e0880ae86baad2
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08071597B2

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