Benzyl Bromide → 2-Benzyloxy-4,5-difluoronitrobenzene

HRID 660831노트

반응식

HRID 660831 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([OH:9])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:19](Br)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CC(C)=O>[CH2:19]([O:9][C:5]1[CH:6]=[C:7]([F:8])[C:2]([F:1])=[CH:3][C:4]=1[N+:10]([O-:12])=[O:11])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 27741824,5-Difluoro-2-nitrophenol

생성물 1

HCID 688400302-Benzyloxy-4,5-difluoronitrobenzene

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a vigorously stirred mixture of 4,5-difluoro-2-nitrophenol (1 g, 5.71 mmol) and anhydrous potassium carbonate (1.9 g, 14.28 mmol) in acetone (20 mL). is added benzyl bromide (750 μl, 6.28 mmol) and the dark heterogeneous mixture is heated to reflux for 10 h; or until all starting material had been consumed according to LC/MS analysis. The dark mixture is then filtered, dried over magnesium sulfate, and filtered again to afford, after solvent removal, a light brown crystalline solid that was used in the next step without further purification.

후처리

  1. temperaturethe dark heterogeneous mixture is heated
  2. temperatureto reflux for 10 h
  3. customor until all starting material had been consumed
  4. filtrationThe dark mixture is then filtered
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered again
  7. customto afford
  8. customafter solvent removal
  9. customa light brown crystalline solid that was used in the next step without further purification

출처 및 근거

ORD 기록
ord-e27f13424c964523a059667bbc9feb36
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084448B2

반응 노트

불러오는 중…