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Dimethylformamide → 4-Bromo-2,5-difluorobenzaldehyde

HRID 516547
ノート
印刷プレビュー

反応式

HRID 516547 の反応式
Br[C:2]1[CH:7]=[C:6]([F:8])[C:5]([Br:9])=[CH:4][C:3]=1[F:10].C([Li])CCC.CN([CH:19]=[O:20])C>C(OCC)C>[Br:9][C:5]1[C:6]([F:8])=[CH:7][C:2]([CH:19]=[O:20])=[C:3]([F:10])[CH:4]=1
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

5

反応物 3

HCID 6228DimethylformamideHCID 675961,4-Dibromo-2,5-difluorobenzeneHCID 178418339Butyllithium

生成物 1

HCID 224890814-Bromo-2,5-difluorobenzaldehyde収率 86.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
-78 °C

実験手順

To a solution of 2,5-dibromo-1,4-difluorobenzene (10.0 g, 36.77 mmol) in diethyl ether (150 mL) at −78° C. was added n-butyl lithium (2.5 M in Hexanes, 14.86 mL, 37.15 mmol) dropwise under nitrogen. The reaction mixture was stirred at −78° C. for 30 min. Dry DMF (3.13 mL, 40.46 mmol) in diethyl ether (10 mL) was added dropwise and reaction was slowly warmed to room temperature over 2 h. The reaction was quenched with aqueous saturated ammonium chloride solution (25 mL) and extracted with diethyl ether. The organic phase was washed with saturated brine solution, dried (Na2SO4), filtered, and concentrated under reduced pressure (Note: Product is highly volatile). The crude product was purified by flash chromatography (SiO2, eluting with 2-20% ethyl acetate in hexanes) to provide the title compound as a pale yellow solid (7.0 g, 86%): 1H NMR (400 MHz, CDCl3): δ 7.50 (dd, J=5.08, 8.92 Hz, 1H), 7.62 (dd, J=5.80, 7.68 Hz, 1H), 10.30 (d, J=2.76 Hz, 1H).

後処理

  1. customreaction
  2. temperaturewas slowly warmed to room temperature over 2 h
  3. customThe reaction was quenched with aqueous saturated ammonium chloride solution (25 mL)
  4. extractionextracted with diethyl ether
  5. washThe organic phase was washed with saturated brine solution
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure (
  9. customThe crude product was purified by flash chromatography (SiO2, eluting with 2-20% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-afdf9c10bed24658ac63f0682cfb338e
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09113629B2

反応ノート

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