Ethyl Acetate → 4-Fluoro-2,5-dimethylphenol

HRID 278049노트

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HRID 278049 반응식
[F:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([O:9]C)=[C:4]([CH3:11])[CH:3]=1.B(Br)(Br)Br.C(OCC)(=O)C>ClCCl>[F:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[C:4]([CH3:11])[CH:3]=1

참가 물질

5

실험 절차

9.7 g of 4-fluoro-2,5-dimethylanisol was dissolved in 100 ml of dichloromethane and 76 ml of boron tribromide (1.0M dichloromethane solution) was added to the solution at 0° C. The resulting mixture was brought to room temperature, stirred for one hour, and poured into ice-water. 300 ml of ethyl acetate was added to the resultling mixture. The organic layer was washed with water, a saturated aqueous solution of sodium bicarbonate and brine successively, dried over magnesium sulfate. After the desiccant was filtered off, the resulting mixture was evaporated. The resulting crude product was purified by silica gel column chromatography to give 8.5 g of the title compound as a pale brown oil.

후처리

  1. customwas brought to room temperature
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium bicarbonate and brine successively, dried over magnesium sulfate
  4. filtrationAfter the desiccant was filtered off
  5. customthe resulting mixture was evaporated
  6. customThe resulting crude product was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-d6a714e4fe5344f3ab2c513c68e6cbb5
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06358995B1

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