Tert-Butyl nitrite → HCID 14651251, Verbindung

HRID 232648Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 232648
N(OC(C)(C)C)=O.[F:8][C:9]1[C:15]([CH3:16])=[C:14]([F:17])[C:13]([F:18])=[C:12]([CH3:19])[C:10]=1N>CN(C)C=O>[F:18][C:13]1[C:14]([F:17])=[C:15]([CH3:16])[C:9]([F:8])=[CH:10][C:12]=1[CH3:19]

Komponenten

4

Edukt 2

HCID 10906Tert-Butyl nitriteHCID 23359007HCID 23359007, Verbindung

Produkt 1

HCID 14651251HCID 14651251, VerbindungAusbeute 49 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

A solution of t-butyl nitrite (4.56 g) in anhydrous dimethylformamide (26.5 ml) is stirred with heating at 50°-52° C. and thereto a solution of 2,4,5-trifluoro-3,6-dimethylaniline (4.24 g) in anhydrous dimethylformamide (40 ml) is added dropwise at 50°-52° C. over a period of 30 minutes. The mixture is further stirred at the same temperature for 30 minutes. After cooling, the mixture is poured into ice-water, extracted with diethyl ether, and the extract is washed with water, and then with diluted hydrochloric acid and dried. The diethyl ether is distilled off under atomospheric pressure and the residue is concentrated and distilled under atomospheric pressure to give 2,3,5-trifluoro-4-methyltoluene (1.9 g), as yellow oil, b.p. 120°-125° C.

Aufarbeitung

  1. temperaturewith heating at 50°-52° C.
  2. temperatureAfter cooling
  3. extractionextracted with diethyl ether
  4. washthe extract is washed with water
  5. dry with materialwith diluted hydrochloric acid and dried
  6. distillationThe diethyl ether is distilled off under atomospheric pressure
  7. concentrationthe residue is concentrated
  8. distillationdistilled under atomospheric pressure

Quellen und Nachweise

ORD-Eintrag
ord-ebcf91937c4246739a04427c37bb4391
Quelldatensatz
uspto-grants-1997_01
Patentnummer
US05591744

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