反応 #93299

反応方程式

2-(2,4-dichlorophenyl)-1-(4-fluorophenyl)-3-(1H-1,2,4-triazol-1-yl)-1,2-propanediol

1,1'-carbonyldiimidazole

chloroform

→

4-(2,4-dichlorophenyl)-5-(4-fluorophenyl)-2-oxo-4-(1H-1,2,4-triazol-1-yl)methyl-1,3-dioxolane

収率 78.7%

溶媒

Water

反応条件

後処理

1. 1
   温度is heated
2. 2
   温度under reflux for 1 hour
3. 3
   その他the chloroform layer is separated
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   濃縮concentrated
6. 6
   その他The residue is chromatographed on a column of silica-gel
7. 7
   洗浄eluted with a mixture of methylene chloride and methanol (100:0-98:2 v/v)
8. 8
   濃縮The eluate is concentrated
9. 9
   その他the residue is crystallized from ethyl acetate-isopropyl ether

実験手順

A mixture of 500 mg of 2-(2,4-dichlorophenyl)-1-(4-fluorophenyl)-3-(1H-1,2,4-triazol-1-yl)-1,2-propanediol, 530 mg of 1,1'-carbonyldiimidazole and 10 ml of dry chloroform is heated under reflux for 1 hour. Water is added to the reaction mixture, and the chloroform layer is separated, dried over anhydrous sodium sulfate, and concentrated. The residue is chromatographed on a column of silica-gel and eluted with a mixture of methylene chloride and methanol (100:0-98:2 v/v). The eluate is concentrated, and the residue is crystallized from ethyl acetate-isopropyl ether to give 420 mg of 4-(2,4-dichlorophenyl)-5-(4-fluorophenyl)-2-oxo-4-(1H-1,2,4-triazol-1-yl)methyl-1,3-dioxolane as crystals. m.p. 191°-192° C. Yield: 78.7%

出典