반응 #52184

반응 방정식

sodium hydroxide

diethyl 2-(2,4,6-trifluorophenyl)malonate

triethylamine

3-amino-1,2,4-triazole

→

5,7-dihydroxy-6-(2,4,6-trifluorophenyl)-1,2,4-triazolo[1,5-a]pyrimidine

용매

water

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도The reaction mixture was then cooled to 50° C.
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   세척The aqueous phase was washed with ether
5. 5
   여과The precipitated colorless solid was filtered off
6. 6
   세척washed with water and diisopropyl ether
7. 7
   기타dried

실험 절차

A mixture of 22 mmol of diethyl 2-(2,4,6-trifluorophenyl)malonate, 24 mmol of triethylamine and 22 mmol of 3-amino-1,2,4-triazole was heated with stirring at 180° C. for 6 hours. The reaction mixture was then cooled to 50° C., admixed with a solution of 2.2 g of sodium hydroxide in 25 ml of water and stirred for 30 minutes. The aqueous phase was washed with ether and then acidified with conc. hydrochloric acid. The precipitated colorless solid was filtered off, washed with water and diisopropyl ether and dried. The yield of the title compound was 85% (m.p.: 200-201° C.).

출처