反応 #1045

反応方程式

2,3,3-trifluoro-2-propenyl bromide

triethyl phosphite

→

diethyl (1,1,2-trifluro-2-propenyl)phosphonate

収率 11.0%

diethyl (2,3,3-trifluro-2-propenyl)phosphonate

収率 14.0%

反応条件

後処理

1. 1
   温度at reflux for overnight
2. 2
   その他The residue obtained
3. 3
   その他after evaporation of the solvent
4. 4
   その他was chromatographed over silica gel (hexanes/ethyl acetate/ethanol, 80/20/1)

実験手順

A solution of 2,3,3-trifluoro-2-propenyl bromide (5.25 g, 30 mmol) and triethyl phosphite (4.15 g, 25 mmol) in acetonltrile (15 mL) was heated at reflux for overnight. The residue obtained after evaporation of the solvent was chromatographed over silica gel (hexanes/ethyl acetate/ethanol, 80/20/1) to give diethyl (1,1,2-trifluro-2-propenyl)phosphonate (0.8 g, 11%) and diethyl (2,3,3-trifluro-2-propenyl)phosphonate (1.0 g, 14%).

出典