تفاعل #1960484

ord-1534a6585e12484da63b7f5d73c818ae

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe batch is filtered
  2. 2
    غسيلthe filter residue is washed with MTBE
  3. 3
    أخرىThe filtrate is evaporated to dryness
  4. 4
    أخرىthe residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1)

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08303844B2uspto-grants-2012_11