Reaktion #1807147
ord-7da07ea2dfe048e3acb2d300216efd35
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe resulting crystals were collected
- 2Waschenwashed with water
- 3Sonstigedried
- 4SonstigeThe crude crystals were chromatographed on silica gel with 20% ethyl acetate-chloroform
- 5Sonstigerecrystallized from a mixture of ethyl acetate, chloroform and hexane
Vorschrift
A mixture of 4-amino-6-(2-ethylbutyramido)-quinazoline (0.9 g) and diethyl ethoxymethylenepropanedioate (0.95 g) in N,N-dimethylformamide (4 ml) was stirred at 100° C. for 2 hours and 40 minutes. Water was added to the reaction mixture. The resulting crystals were collected, washed with water and dried. The crude crystals were chromatographed on silica gel with 20% ethyl acetate-chloroform and recrystallized from a mixture of ethyl acetate, chloroform and hexane to give crystalline diethyl [[6-(2-ethylbutyramido)-4-quinazolinylamino]methylene]propanedioate (1.1 g).