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

HRID 389105
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HRID 389105 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 58243772HCID 58243772, 화합물

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ce1b9ca879cd487db3d9156d8737486e
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08377923B2

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