反応 #336543

反応方程式

water

p-phenoxyphenol

potassium carbonate

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

→

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

収率 30.9%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   抽出extracted three times with ethyl acetate
2. 2
   乾燥The combined organic phases are dried over magnesium sulfate
3. 3
   濃縮concentrated
4. 4
   その他The residue is purified by chromatography over silica gel

実験手順

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.

出典