反応 #426696

ord-12596ad63e034068bc35439fa725b6d2

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to rise to room temperature
  2. 2
    workup.STIRRINGstirred for 48 h
  3. 3
    その他The solvent was removed under reduced pressure
  4. 4
    その他the residue was purified by flash chromatography (5:1 DCM/Hexane)

実験手順

To a mixture of 4-hydroxybenzaldehyde (1.45 g, 11.9 mmol), triphenylphosphine (6.87 g, 26.2 mmol) and 2-fluoroethanol (1.68 g, 26.2 mmol) in dry THF (70 ml) at 0° C., was added DIAD (5.29 g, 26.2 mmol) dropwise. The reaction mixture was stirred at 0° C. for 1 h then allowed to rise to room temperature and stirred for 48 h. The solvent was removed under reduced pressure and the residue was purified by flash chromatography (5:1 DCM/Hexane) to give the title compound (0.807 g, 40%) as a colourless solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08895313B2uspto-grants-2014_11