Benzyl Chloride → 4-Bromo-2,6-difluoro-1-(benzyloxy)benzene

HRID 579907

反応式

HRID 579907 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([OH:9])=[C:4]([F:10])[CH:3]=1.[CH2:11](Cl)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>>[CH2:11]([O:9][C:5]1[C:6]([F:8])=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[F:10])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

4

反応物 3

HCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 27362924-Bromo-2,6-difluorophenol

生成物 1

HCID 142076414-Bromo-2,6-difluoro-1-(benzyloxy)benzene

実験手順

A stirred mixture of 4-bromo-2,6-difluorophenol (36 g, 0.172 mole), benzylchloride (21.77 g, 0.172 mole), and potassium carbonate (25 g, 0.18 mole) in demethylformamide (300 ml) was heated at 80°-90° for four hours. After cooling, the solvent was evaporated and ether added to the residue. The insoluble inorganic salts were removed by filtration, and solvent evaporated from the filtrate. The oily residue was subjected to bulb-to-bulb vacuum distillation on Kugelrohr apparatus to give the desired product as a nearly colorless oil (41 g, 80 percent): R.I.=1.5602 @ 25° C.; NMR (CDCl3) was consistent with the assigned structure.

後処理

  1. temperaturewas heated at 80°-90° for four hours
  2. temperatureAfter cooling
  3. customthe solvent was evaporated
  4. additionether added to the residue
  5. customThe insoluble inorganic salts were removed by filtration, and solvent
  6. customevaporated from the filtrate
  7. distillationThe oily residue was subjected to bulb-to-bulb vacuum distillation on Kugelrohr apparatus

出典と根拠

ORDレコード
ord-1e7166d355f54776891f441e1a93fe78
出典データセット
uspto-grants-1988_06
特許番号
US04750931

関連ノート

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