Sulfuric Acid → 3,5-Difluoro-2-nitrobenzonitrile

HRID 1092249

Reaktionsgleichung

Reaktionsgleichung von HRID 1092249
[N+:1]([O-:4])([O-])=[O:2].[K+].OS(O)(=O)=O.[F:11][C:12]1[CH:13]=[C:14]([CH:17]=[C:18]([F:20])[CH:19]=1)[C:15]#[N:16]>>[F:11][C:12]1[C:13]([N+:1]([O-:4])=[O:2])=[C:14]([CH:17]=[C:18]([F:20])[CH:19]=1)[C:15]#[N:16]

Komponenten

4

Edukt 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 5872043,5-Difluorobenzonitrile

Produkt 1

HCID 545943353,5-Difluoro-2-nitrobenzonitrileAusbeute 95,4 %

Versuchsvorschrift

Potassium nitrate (6.56 g, 64.8 mmol) was added to concentrated H2SO4 (33.7 ml, 633 mmol) at 0° C., followed by slow addition of 3,5-difluorobenzonitrile (4.4 g, 31.6 mmol). The suspension was stirred at this temperature for an additional 3 hours and quenched with ice water (500 ml). The resulting solid was collected by filtration and dried to give the title compound (5.55 g, 95%) as a white solid. 1H NMR (400 MHz, CDCl3) 7.43 (m, 1H), 7.35 (m, 1H).

Aufarbeitung

  1. customquenched with ice water (500 ml)
  2. filtrationThe resulting solid was collected by filtration
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f555e6cb619a4592bc23723a8bcc8aa1
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08129403B2

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