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Cesium carbonate → 1-Bromo-3-fluoro-5-propoxybenzene

HRID 20435
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HRID 20435 반응식
[CH2:1](I)[CH2:2][CH3:3].[Br:5][C:6]1[CH:7]=[C:8]([OH:13])[CH:9]=[C:10]([F:12])[CH:11]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[Br:5][C:6]1[CH:7]=[C:8]([O:13][CH2:1][CH2:2][CH3:3])[CH:9]=[C:10]([F:12])[CH:11]=1
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참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 336431-IodopropaneHCID 219046363-Bromo-5-fluorophenol

생성물 1

HCID 685580051-Bromo-3-fluoro-5-propoxybenzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Add propyl iodide (5.74 g, 33.77 mmol) to 3-bromo-5-fluoro-phenol (4.30 g, 22.51 mmol) and cesium carbonate (11.00 g, 33.77 mmol) in N,N-dimethylformamide (75 mL) and stir at room temperature 1 hour, then heat at 50° C. for 1 hour. Cool to room temperature and dilute with hexanes. Wash (water, 1N lithium chloride, saturated aqueous sodium chloride), dry (magnesium sulfate), filter and concentrate to give the desired compound as a colorless oil, 4.40 g (83.8%).

후처리

  1. temperatureheat at 50° C. for 1 hour
  2. temperatureCool to room temperature
  3. washWash (water, 1N lithium chloride, saturated aqueous sodium chloride)
  4. dry with materialdry (magnesium sulfate)
  5. filtrationfilter
  6. concentrationconcentrate

출처 및 근거

ORD 기록
ord-eb96c5088f05479f886160d7fefef98d
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745438B2

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