Réaction #1960484

ord-1534a6585e12484da63b7f5d73c818ae

Équation de réaction

Oc1cccc(F)c1F
2,3-difluorophenol
C#CCBr
propargyl bromide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
C#CCOc1cccc(F)c1F
1,2-difluoro-3-prop-2-ynyloxybenzene

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    FiltrationThe batch is filtered
  2. 2
    Lavagethe filter residue is washed with MTBE
  3. 3
    AutreThe filtrate is evaporated to dryness
  4. 4
    Autrethe residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1)

Mode opératoire

115.0 g (0.88 mol) of 2,3-difluorophenol are refluxed for 3 h in 1.6 l of ethyl methyl ketone together with 118.2 ml (17.7 mol) of propargyl bromide (80% soln. in toluene) and 146.6 g (138.2 mol) of potassium carbonate. The batch is filtered, and the filter residue is washed with MTBE. The filtrate is evaporated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08303844B2uspto-grants-2012_11