Reaktion #486566

Reaktionsgleichung

4-amino-3-pyridinol

N,N-dimethylformamide dimethyl acetal

→

4-[[(Dimethylamino)methylene]amino]-3-pyridinol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 30 minutes
2. 2
   EinengenAt the end of this time, the reaction mixture was concentrated under reduced pressure
3. 3
   Wascheneluting with 5% methanol/ethyl acetate
4. 4
   EinengenThe eluate was concentrated
5. 5
   Sonstigethe residue and recrystallized from ethyl acetate/pentane
6. 6
   Sonstigeto afford 0.91 g of analytically pure product, m.p. 121°-123°

Vorschrift

A solution prepared from of 4-amino-3-pyridinol (1.10 g) and 10 ml of N,N-dimethylformamide dimethyl acetal was refluxed for 30 minutes. At the end of this time, the reaction mixture was concentrated under reduced pressure and the residue was passed over a short column of florisil, eluting with 5% methanol/ethyl acetate. The eluate was concentrated and the residue and recrystallized from ethyl acetate/pentane to afford 0.91 g of analytically pure product, m.p. 121°-123°.

Quelle