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2-Nitrobenzoyl chloride → N-[4-bromo-3-(trifluoromethyl)phenyl]-2-nitrobenzamide

HRID 8897
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 8897
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:5]([Br:8])=[CH:6][CH:7]=1.[OH-].[Na+].[N+:15]([C:18]1[CH:26]=[CH:25][CH:24]=[CH:23][C:19]=1[C:20](Cl)=[O:21])([O-:17])=[O:16]>C(OCC)(=O)C>[N+:15]([C:18]1[CH:26]=[CH:25][CH:24]=[CH:23][C:19]=1[C:20]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[C:4]([C:9]([F:12])([F:10])[F:11])[CH:3]=1)=[O:21])([O-:17])=[O:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 118752-Nitrobenzoyl chlorideHCID 14798Sodium HydroxideHCID 678524-Bromo-3-(trifluoromethyl)aniline

Produkt 1

HCID 1300995N-[4-bromo-3-(trifluoromethyl)phenyl]-2-nitrobenzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

A solution of 3-amino-6-bromobenzotrifluoride (Fluka, Buchs, Switzerland; 24.0 g, 100 mmol) in ethyl acetate (240 mL) is added to a stirred aqueous solution of sodium hydroxide (110 mL of 1 M) at room temperature. This stirred solution is then treated dropwise over 30 minutes with a solution of 2-nitrobenzoyl chloride (Fluka, Buchs, Switzerland; 14.5 mL, 110 mmol) in ethyl acetate (150 mL). The resulting mixture is then stirred for 30 min at ambient temperature. The mixture is extracted with ethyl acetate (3×100 mL) and the combined extracts are sequentially washed with hydrochloric acid (2×100 mL of 2M), water (2×100 mL), saturated aqueous sodium hydrogen carbonate solution (2×100 mL) and saturated aqueous sodium chloride (1×100 mL), dried (MgSO4), filtered and the solvent is evaporated under reduced pressure to yield the crude product which is purified by recrystallisation from ethyl acetate-hexane to give the title compound as a beige crystalline solid, m.p. 157–158° C.

Aufarbeitung

  1. extractionThe mixture is extracted with ethyl acetate (3×100 mL)
  2. washthe combined extracts are sequentially washed with hydrochloric acid (2×100 mL of 2M), water (2×100 mL), saturated aqueous sodium hydrogen carbonate solution (2×100 mL) and saturated aqueous sodium chloride (1×100 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent is evaporated under reduced pressure
  6. customto yield the crude product which
  7. customis purified by recrystallisation from ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-08f8d6788814465f87faa5aa3662b783
Quelldatensatz
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07091224B2

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