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

HRID 53810

Reaktionsgleichung

Reaktionsgleichung von HRID 53810
[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); δ 7.141 (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-5b65582b6713465381b61a73f53f9b59
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05620979

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