Methanol → Methyl 2-fluoro-4-methoxybenzoate

HRID 553625노트

반응식

HRID 553625 반응식
[F:1][C:2]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(Cl)(Cl)=O.[CH3:17]O>>[CH3:17][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:2]=1[F:1]

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 27745422-Fluoro-4-methoxybenzoic acid

생성물 1

HCID 21255685Methyl 2-fluoro-4-methoxybenzoate수율 92%

실험 절차

To a solution of 5.0 g (29.4 mmol) of 2-fluoro-4-methoxybenzoic acid in methanol (50 mL) at room temperature are added 2.13 mL (29.4 mmol) of thionyl chloride. The reaction is stirred at room temperature for 16 h and the solvent is removed under reduced pressure. The residue is dissolved in DCM and washed with brine. The organic layer is dried (MgSO4), filtered and the filtrate is concentrated under reduced pressure to give 5.04 g (27.1 mmol) of 2-fluoro-4-methoxybenzoic acid methyl ester. Yield: 92%, ES-MS: m/z 185 [M+H].

후처리

  1. customthe solvent is removed under reduced pressure
  2. dissolutionThe residue is dissolved in DCM
  3. washwashed with brine
  4. dry with materialThe organic layer is dried (MgSO4)
  5. filtrationfiltered
  6. concentrationthe filtrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3c50191659da43d788b315dc6e5748d7
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048899B2

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