Reaktion #448507

Reaktionsgleichung

4-amino-3-pyridinol

N,N-diethylformamide dimethyl acetal

→

crystalline solid

Ausbeute 61.5%

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

Ausbeute 61.5%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated under nitrogen for 2 hours
2. 2
   EinengenThe solution was concentrated under reduced pressure
3. 3
   FiltrationThe resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran
4. 4
   Sonstigeto give a solid
5. 5
   SonstigeRecrystallization of the purified product from ethyl acetate/hexanes

Vorschrift

A mixture of 4-amino-3-pyridinol (3.90 g), N,N-diethylformamide dimethyl acetal (11.68 g) and toluene (20 mL) was heated under nitrogen for 2 hours. The solution was concentrated under reduced pressure. The resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran to give a solid. Recrystallization of the purified product from ethyl acetate/hexanes afforded 4.21 g of crystalline solid, m.p. 104°-106° C.

Quelle