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Sodium Chloride → 2-Bromo-1-(2,4-difluorophenoxy)-4-nitrobenzene

HRID 930858
ノート
印刷プレビュー

反応式

HRID 930858 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1F.[F:12][C:13]1[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=1[OH:20].C(=O)([O-])[O-].[Cs+].[Cs+].[Cl-].[Na+]>CS(C)=O.O>[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[O:20][C:14]1[CH:15]=[CH:16][C:17]([F:19])=[CH:18][C:13]=1[F:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5234Sodium ChlorideHCID 10796Cesium carbonateHCID 696992-Bromo-1-fluoro-4-nitrobenzeneHCID 1230512,4-Difluorophenol

生成物 1

HCID 867049232-Bromo-1-(2,4-difluorophenoxy)-4-nitrobenzene収率 100.2%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide
溶媒
HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

A mixture of 2-bromo-1-fluoro-4-nitrobenzene (15 g, 68 mmol), 2,4-difluorophenol (7.82 ml, 82 mmol), and cesium carbonate (26.7 g, 82 mmol) in dimethylsulfoxide (75 mL) was heated to 110° C. for 1 hour. The reaction mixture was cooled to ambient temperature and water (1000 mL) and saturated aqueous sodium chloride (1000 mL) were added. The mixture was extracted with ethyl acetate (3×200 mL). The combined organics were washed with saturated aqueous sodium chloride, dried (anhydrous magnesium sulfate), filtered, and concentrated under reduced pressure to provide the title compound (22.5 g, quantitative).

後処理

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. extractionThe mixture was extracted with ethyl acetate (3×200 mL)
  3. washThe combined organics were washed with saturated aqueous sodium chloride
  4. dry with materialdried (anhydrous magnesium sulfate)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-79fd50099c3143bd8a393ca065c1eeaf
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296741B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート