反应 #1045

ord-69bdc7c6a2fb4d4987a431b8e37f7f33

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723470uspto-grants-1998_03