반응 #336543

반응 방정식

water

p-phenoxyphenol

potassium carbonate

2-chloro-1-chloromethyl-1,3,4-triazole

→

2-chloro-1-[(p-phenoxyphenoxy)-methyl]-1,3,4-triazole

수율 30.9%

용매

dimethylformamide

반응 조건

후처리

1. 1
   추출extracted three times with ethyl acetate
2. 2
   건조The combined organic phases are dried over magnesium sulfate
3. 3
   농축concentrated
4. 4
   기타The residue is purified by chromatography over silica gel

실험 절차

5.6 g of p-phenoxyphenol and 4.2 g of potassium carbonate are heated for 1 hour at 70° C. in 50 ml of anhydrous dimethylformamide. Subsequently, 5.6 g of 2-chloro-1-chloromethyl-1,3,4-triazole is added and the mixture stirred for 6 hours at 70° C. and overnight at room temperature (about 20° C.). The mixture is then poured into 500 ml of water and extracted three times with ethyl acetate. The combined organic phases are dried over magnesium sulfate and concentrated. The residue is purified by chromatography over silica gel using n-hexane/ethyl acetate (2:1) as eluant. There is obtained 2.8 g of 2-chloro-1-[(p-phenoxyphenoxy)-methyl]-1,3,4-triazole as an oil.

출처