Water → 1,4-Dimethyl-2-nitro-5-[3-(trifluoromethyl)phenoxy]benzene

HRID 431078

Reaktionsgleichung

Reaktionsgleichung von HRID 431078
[H-].[Na+].[F:3][C:4]([F:13])([F:12])[C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1.Cl[C:15]1[CH:16]=[C:17]([CH3:25])[C:18]([N+:22]([O-:24])=[O:23])=[CH:19][C:20]=1[CH3:21].O>CN1CCCC1=O>[N+:22]([C:18]1[CH:19]=[C:20]([CH3:21])[C:15]([O:11][C:7]2[CH:8]=[CH:9][CH:10]=[C:5]([C:4]([F:12])([F:13])[F:3])[CH:6]=2)=[CH:16][C:17]=1[CH3:25])([O-:24])=[O:23]

Komponenten

6

Edukt 4

HCID 962WaterHCID 73763-(Trifluoromethyl)phenolHCID 24758Sodium hydrideHCID 2527931-Chloro-2,5-dimethyl-4-nitrobenzene

Produkt 1

HCID 155400711,4-Dimethyl-2-nitro-5-[3-(trifluoromethyl)phenoxy]benzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a suspension of sodium hydride (0.4 g of 60% in oil) in dry N-methylpyrroli-dinone (10 ml) was slowly added 3-trifluoromethylphenol (1.62 g). When effervescence had ceased, 3-chloro-6-nitro-p-xylene (1.85 g) was added and the mixture stirred at 120-40° C. for 5 hours. On cooling, the mixture was poured into water and the mixture extracted with diethyl ether (x3). The combined ether extracts were dried (MgSO4), filtered and evaporated to give the title compound as a solid, m.p. 68-71° C.

Aufarbeitung

  1. temperatureOn cooling
  2. extractionthe mixture extracted with diethyl ether (x3)
  3. dry with materialThe combined ether extracts were dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f250edac67b04269b8718383f2b709f6
Quelldatensatz
uspto-grants-2003_12
Patentnummer
US06656967B2

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