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Water → Dimethyl 2-fluoro-5-methylbenzene-1,4-dicarboxylate

HRID 389105
ノート
印刷プレビュー

反応式

HRID 389105 の反応式
[C:1](=O)([O-])[O-].[K+].[K+].IC.[F:9][C:10]1[CH:18]=[C:17]([C:19](O)=[O:20])[C:16]([CH3:22])=[CH:15][C:11]=1[C:12]([OH:14])=[O:13].O.CN([CH:27]=[O:28])C>>[F:9][C:10]1[CH:18]=[C:17]([C:19]([O:28][CH3:27])=[O:20])[C:16]([CH3:22])=[CH:15][C:11]=1[C:12]([O:14][CH3:1])=[O:13]
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 5

HCID 962WaterHCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 58243772HCID 58243772、化合物

生成物 1

HCID 56965483Dimethyl 2-fluoro-5-methylbenzene-1,4-dicarboxylate

実験手順

Potassium carbonate (1.2 g) and iodomethane (0.7 ml) were added to a solution of 2-fluoro-5-methylterephthalic acid (755 mg) in DMF (5 ml), followed by stirring at room temperature overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was further washed with water and then saturated brine, the solvent was evaporated under reduced pressure, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 90:10), and the solvent was evaporated under reduced pressure to obtain, as a colorless solid, dimethyl 2-fluoro-5-methylterephthalate (708 mg).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was further washed with water
  3. customsaturated brine, the solvent was evaporated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 90:10)
  5. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ce1b9ca879cd487db3d9156d8737486e
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08377923B2

反応ノート

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