Propargyl bromide → 5-Bromo-1,2-difluoro-3-prop-2-ynyloxybenzene

HRID 2244844ノート

反応式

HRID 2244844 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([F:10])[C:5]([F:9])=[C:6]([OH:8])[CH:7]=1.[CH2:11](Br)[C:12]#[CH:13].C(=O)([O-])[O-].[K+].[K+]>CC(CC)=O>[Br:1][C:2]1[CH:7]=[C:6]([O:8][CH2:13][C:12]#[CH:11])[C:5]([F:9])=[C:4]([F:10])[CH:3]=1

参加物

5

反応物 3

HCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 27733075-Bromo-2,3-Difluorophenol

生成物 1

HCID 592152525-Bromo-1,2-difluoro-3-prop-2-ynyloxybenzene

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

50.0 g (0.24 mol) of 5-bromo-2,3-difluorophenol are refluxed for 3 h together with 32.0 ml (0.29 mol) of propargyl bromide (80% soln. in toluene) and 39.7 g (0.29 mol) of potassium carbonate in 860 ml of ethyl methyl ketone. The batch is filtered, and the filter residue is washed with MTBE. The filtrate is concentrated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1).

後処理

  1. filtrationThe batch is filtered
  2. washthe filter residue is washed with MTBE
  3. concentrationThe filtrate is concentrated to dryness
  4. customthe residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1)

出典と根拠

ORDレコード
ord-bb35b0ddd6654b0c9dc938195de1d6ce
出典データセット
uspto-grants-2010_03
特許番号
US07678929B2

反応ノート

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