Phosphorus tribromide → 4-Bromo-2-(bromomethyl)-1-fluorobenzene

HRID 563786

반응식

HRID 563786 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:8]O)[CH:7]=1.P(Br)(Br)[Br:12].C([O-])(O)=O.[Na+]>COCCOC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:8][Br:12])[CH:7]=1

참가 물질

5

반응물 3

HCID 24614Phosphorus tribromideHCID 516892Sodium BicarbonateHCID 2773352(5-Bromo-2-fluorophenyl)methanol

생성물 1

HCID 135532954-Bromo-2-(bromomethyl)-1-fluorobenzene

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

To (5-bromo-2-fluoro-phenyl)-methanol (1.2 g, 5.9 mmol) in DME (20 mL) was added phosphorus tribromide (0.83 mL, 8.8 mmol), and the reaction was stirred at room temperature for 6 hours. The mixture was cooled to 0° C. and adjusted to pH 6 with saturated aqueous NaHCO3. The solution was extracted with EtOAc, and the combined organic layers were dried, concentrated, and purified by silica gel chromatography to give the title compound.

후처리

  1. temperatureThe mixture was cooled to 0° C.
  2. extractionThe solution was extracted with EtOAc
  3. customthe combined organic layers were dried
  4. concentrationconcentrated
  5. custompurified by silica gel chromatography

출처 및 근거

ORD 기록
ord-81d61cfb8f294986860eb236a730ea7e
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067445B2

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