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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
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 358868
[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]
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Komponenten

4

Edukt 2

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-aadd31a63e784190b9647379efa783e7
Quelldatensatz
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04997943

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