Reaktion #442078

Reaktionsgleichung

4-amino-6-(2-ethylbutyramido)quinazoline

diethyl ethoxymethylenepropanedioate

Water

→

diethyl [[6-(2-ethylbutyramido)-4-quinazolinylamino]methylene]propanedioate

Ausbeute 73.7%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe resulting crystals were collected
2. 2
   Waschenwashed with water
3. 3
   Sonstigedried
4. 4
   SonstigeThe crude crystals were chromatographed on silica gel with 20% ethyl acetate-chloroform
5. 5
   Sonstigerecrystallized 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).

Quelle