Ethanol → Ethyl 4-fluoro-2-hydroxybenzoate

HRID 73317

반응식

HRID 73317 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([OH:11])[CH:3]=1.S(Cl)(Cl)=O.[CH2:16](O)[CH3:17]>>[CH2:16]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([F:1])=[CH:3][C:4]=1[OH:11])[CH3:17]

참가 물질

4

반응물 3

HCID 702EthanolHCID 24386Thionyl ChlorideHCID 676614-Fluorosalicylic acid

생성물 1

HCID 22478444Ethyl 4-fluoro-2-hydroxybenzoate

실험 절차

To a solution of 4-fluoro-2-hydroxybenzoic acid (3.0 g) in ethanol (40 mL) was added thionyl chloride (5.61 mL) at 0° C., and the mixture was heated under reflux for 24 hours. The reaction mixture was concentrated under reduced pressure. This residue was poured into water, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (3.5 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 24 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionThis residue was poured into water
  5. extractionthe resulting mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with water and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-7659cbae769d450f8f537268ffb4e0b9
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829040B2

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