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Methyl iodide → Methyl 3-fluoro-2-methylbenzoate

HRID 2301125
ノート
印刷プレビュー

反応式

HRID 2301125 の反応式
[F:1][C:2]1[C:3]([CH3:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[C:12](=O)([O-])[O-].[K+].[K+].CI.C(OCC)(=O)C>CN(C)C=O>[CH3:12][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][CH:10]=[C:2]([F:1])[C:3]=1[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 2466823-Fluoro-2-methylbenzoic acid

生成物 1

HCID 21752566Methyl 3-fluoro-2-methylbenzoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-Fluoro-2-methyl-benzoic acid (4.8 g, 31 mmol), potassium carbonate (4.3 g, 31 mmol) and methyl iodide (4.5 g, 31 mmol) were stirred at room temperature for 17.5 hours in anhydrous N,N-dimethylformamide (50 ml). The reaction solution was mixed with ethyl acetate, washed with water and saturated brine and then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation from the organic, layer under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 4.8 g (27 mmol, 87% in yield) of the title compound.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. washwashed with water and saturated brine
  2. dry with materialdried with anhydrous magnesium sulfate
  3. customThe solvent was removed by evaporation from the organic, layer under a reduced pressure
  4. customthe thus obtained material was separated
  5. custompurified by a silica gel column chromatography
  6. customto obtain

出典と根拠

ORDレコード
ord-6f10e80fff854466bb6addb329ad0ddd
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06498251B1

反応ノート

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