Reaktion #155720

Reaktionsgleichung

Intermediate b

ethyl[2-cyano-2-(2-phenylhydrazono)acetamido]formate

sodium acetate

acetic acid

→

solid

Ausbeute 70.0%

2-phenyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

Ausbeute 70.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was warmed up
2. 2
   Sonstigeto react
3. 3
   Temperaturunder reflux for 2 h
4. 4
   SonstigeAfter completion of the reaction
5. 5
   Filtrationfiltered by suction
6. 6
   WaschenThe filtered cake was washed with water and petroleum ether
7. 7
   Sonstigedried

Vorschrift

Intermediate b (21 g, 0.08 mol) and anhydrous sodium acetate (29 g, 0.35 mol) were added to glacial acetic acid (20v/w, 420 mL). The mixture was warmed up to react under reflux for 2 h. After completion of the reaction, the reaction solution was cooled to 0° C. and poured into water (1200 mL). The mixture was stirred for 30 min and filtered by suction. The filtered cake was washed with water and petroleum ether, and dried to produce an orange red solid (12 g) in a yield of 67.8%.

Quelle