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Potassium Hydroxide → 4-Bromo-2-chloro-1-(difluoromethoxy)benzene

HRID 70577
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HRID 70577 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([Cl:9])[CH:3]=1.[OH-].[K+].Cl[C:13]([F:23])([F:22])C(C1C=CC=CC=1)=O>C(#N)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:13]([F:23])[F:22])=[C:4]([Cl:9])[CH:3]=1
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참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 198594-Bromo-2-chlorophenolHCID 2382962-Chloro-2,2-difluoroacetophenone

생성물 1

HCID 463115384-Bromo-2-chloro-1-(difluoromethoxy)benzene수율 52%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
80 °C

실험 절차

A solution of 4-bromo-2-chlorophenol (830 mg) and a 30% potassium hydroxide solution (16 mL) in acetonitrile (16 mL) was cooled to −78° C. 2-Chloro-2,2-difluoroacetophenone (2.95 mL) was added and the mixture was stirred at 80° C. for 40 hours. The reaction solution was cooled to room temperature and extracted with diethyl ether. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1→10:1) to give 4-bromo-2-chloro-1-(difluoromethoxy)benzene as a colorless oil (533 mg, 52%).

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. extractionextracted with diethyl ether
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customThe solvent was then evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1→10:1)

출처 및 근거

ORD 기록
ord-1c82bc8a453045e1bd8067176806964e
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822503B2

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