2-Bromo-3,4-difluoro-1-nitrobenzene → HCID 66751543, Verbindung

HRID 1962880Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1962880
[CH3:1][O-:2].[Na+].[Br:4][C:5]1[C:10]([F:11])=[C:9](F)[CH:8]=[CH:7][C:6]=1[N+:13]([O-:15])=[O:14]>CS(C)=O>[Br:4][C:5]1[C:10]([F:11])=[C:9]([O:2][CH3:1])[CH:8]=[CH:7][C:6]=1[N+:13]([O-:15])=[O:14]

Komponenten

4

Edukt 2

HCID 5745892-Bromo-3,4-difluoro-1-nitrobenzeneHCID 10942334Sodium Methoxide

Produkt 1

HCID 66751543HCID 66751543, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

NaOMe (9.5 g) was added portion wise to a solution of 2-bromo-3,4-difluoro-1-nitro-benzene (21.0 g) dissolved in DMSO (250 ml) at room temperature under nitrogen atmosphere. The mixture was stirred for 3 hrs and then poured onto water and extracted with ethyl acetate. The organic phase was extracted with water and brine, dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product, 2-bromo-3-fluoro-4-methoxy-1-nitro-benzene was used as such in Step 2 described below. 1H NMR (CDCl3) δ ppm: 7.85 (1H, dd); 6.99 (1H, dd); 3.99 (3H, s).

Aufarbeitung

  1. additionpoured onto water
  2. extractionextracted with ethyl acetate
  3. extractionThe organic phase was extracted with water and brine
  4. dry with materialdried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b742a7fc23ff493eb1986406ae538a3e
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08415272B2

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