Potassium Nitrate → 1-Bromo-2,4-difluoro-5-nitrobenzene

HRID 439531

Reaktionsgleichung

Reaktionsgleichung von HRID 439531
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[F:9].[N+:10]([O-])([O-:12])=[O:11].[K+]>OS(O)(=O)=O>[Br:1][C:2]1[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([F:8])=[CH:4][C:3]=1[F:9]

Komponenten

4

Edukt 2

HCID 24434Potassium NitrateHCID 676741-Bromo-2,4-difluorobenzene

Produkt 1

HCID 2230781-Bromo-2,4-difluoro-5-nitrobenzeneAusbeute 91,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
28 °C

Versuchsvorschrift

To a stirred solution of 1-bromo-2,4-difluorobenzene (0.512 g, 2.65 mmol, Aldrich, used as received) in conc. H2SO4 (5.0 mL) at 0° C., KNO3 (0.275 g, 2.72 mmol) was added in one portion. The resulting solution was allowed to warm to 28° C. and was stirred at that temperature overnight. It was then poured into ice (50 g) and extracted with ethylacetate (50 mL). The extract was dried over Na2SO4, and evaporated to afford 0.576 g (91%) pure title compound as light red oil; 1H NMR (CDCl3); δ7.141 (dd, 1H, J1 10.2 Hz, J2 =7.8 Hz), 8.375 (t, 1H, J=7.5 Hz).

Aufarbeitung

  1. extractionextracted with ethylacetate (50 mL)
  2. dry with materialThe extract was dried over Na2SO4
  3. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-745959f1cc00461f8b1ed9db387be198
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05514680

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