Hydrochloric Acid → 3-Bromo-2-methyl-6-nitroaniline

HRID 1411389Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1411389
[Br:1][C:2]1[C:3]([CH3:18])=[C:4]([NH:11]C(=O)C(F)(F)F)[C:5]([N+:8]([O-:10])=[O:9])=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].O.Cl>CO>[Br:1][C:2]1[C:3]([CH3:18])=[C:4]([C:5]([N+:8]([O-:10])=[O:9])=[CH:6][CH:7]=1)[NH2:11]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 73977899N-(3-bromo-2-methyl-6-nitrophenyl)-2,2,2-trifluoroacetamide

Produkt 1

HCID 666306133-Bromo-2-methyl-6-nitroanilineAusbeute 62,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A solution of N-(3-bromo-2-methyl-6-nitrophenyl)-2,2,2-trifluoroacetamide (1.3 g, 3.97 mmol) in CH3OH (30 mL) was treated with potassium carbonate (1.099 g, 7.95 mmol), and the mixture was stirred at 50° C. overnight. The mixture was cooled to room temperature and poured into water, 1N aq HCl was added to adjust to pH 6, and the mixture was extracted with CH2Cl2 (3×). The combined extracts were dried over Na2SO4, and the drying agent was filtered off and solvent was removed in vacuo to give the title compound as a yellow solid (0.57 g, 62%).

Aufarbeitung

  1. temperatureThe mixture was cooled to room temperature
  2. additionwas added
  3. extractionthe mixture was extracted with CH2Cl2 (3×)
  4. dry with materialThe combined extracts were dried over Na2SO4
  5. filtrationthe drying agent was filtered off
  6. customsolvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e53fefba960b4b989a41feac0a33e8a3
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08921514B2

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