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

HRID 331194Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 331194
[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-1686f39fb6664013ac82f03e6c451286
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08877757B2

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