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

HRID 563786

反応式

HRID 563786 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-81d61cfb8f294986860eb236a730ea7e
出典データセット
uspto-grants-2011_11
特許番号
US08067445B2

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