Reaktion #8988

Reaktionsgleichung

(Z)-2-Acetylamino-3-dimethylamino-but-2-enoic acid ethyl ester

cyclopropylamine

→

(Z)-2-Acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester

Lösungsmittel

water

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated under vacuum at 35° C
2. 2
   workup.ADDITIONWater (30 ml) was added to the residue
3. 3
   Sonstigeevaporated again at 35° C
4. 4
   Sonstigeto obtain the desired crude product as a dark brown oil [MS: m/e=227.4 (M+H+)], which
5. 5
   Sonstigecould be used without any further purification for the next step

Vorschrift

(Z)-2-Acetylamino-3-dimethylamino-but-2-enoic acid ethyl ester (4.3 g, 20 mmol) and cyclopropylamine (1.14 g, 20 mmol) were stirred at room temperature in acetic acid (40 ml) for 2 hrs. The reaction mixture was diluted slowly with 30 ml of water and evaporated under vacuum at 35° C. Water (30 ml) was added to the residue and evaporated again at 35° C. The same procedure was repeated twice with toluene (30 ml each) to obtain the desired crude product as a dark brown oil [MS: m/e=227.4 (M+H+)], which could be used without any further purification for the next step.

Quelle