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1,2,4,5-Tetrafluoro-3-methoxy-6-nitrobenzene → 4-Methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene

HRID 358868
ノート
印刷プレビュー

反応式

HRID 358868 の反応式
[C:1]1(=[O:11])[NH:5][C:4](=[O:6])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[K].[CH3:13][O:14][C:15]1[C:20]([F:21])=[C:19](F)[C:18]([N+:23]([O-:25])=[O:24])=[C:17]([F:26])[C:16]=1[F:27]>CN(C)C=O>[CH3:13][O:14][C:15]1[C:16]([F:27])=[C:17]([F:26])[C:18]([N+:23]([O-:25])=[O:24])=[C:19]([N:5]2[C:1](=[O:11])[C:2]3=[CH:10][CH:9]=[CH:8][CH:7]=[C:3]3[C:4]2=[O:6])[C:20]=1[F:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 42613721,2,4,5-Tetrafluoro-3-methoxy-6-nitrobenzeneHCID 24194345Phthalimide potassium salt

生成物 1

HCID 200671344-Methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene収率 60%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.62 g (0.025 mole) of potassium phthalimide were added to a solution of 5.41 g (0.024 mole) of 4-methoxy-2,3,5,6-tetrafluoro-1-nitrobenzene (XXXIII) in 100 ml of dimethylformamide, and the mixture was stirred at room temperature for 3 hours. At the end of this time, the solvent was removed by evaporation under reduced pressure, the residue was dissolved in toluene, and the solution was washed with water, dried and concentrated by evaporation under reduced pressure to give an oily substance. This oily substance was subjected to silica gel column chromatography eluted with toluene, to afford 5.07 g of 4-methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene (XXXIV) as pale yellow powdery crystals.

後処理

  1. customAt the end of this time, the solvent was removed by evaporation under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. washthe solution was washed with water
  4. customdried
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customto give an oily substance
  7. washeluted with toluene

出典と根拠

ORDレコード
ord-aadd31a63e784190b9647379efa783e7
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04997943

反応ノート

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