반응 #155720

반응 방정식

Intermediate b

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

sodium acetate

acetic acid

→

solid

수율 70.0%

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

수율 70.0%

용매

water

반응 조건

후처리

1. 1
   온도The mixture was warmed up
2. 2
   기타to react
3. 3
   온도under reflux for 2 h
4. 4
   기타After completion of the reaction
5. 5
   여과filtered by suction
6. 6
   세척The filtered cake was washed with water and petroleum ether
7. 7
   기타dried

실험 절차

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%.

출처