Nitric Acid → HCID 67272857, Verbindung

HRID 1698600Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1698600
[C:1]([NH:4][C:5]1[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:3])[CH3:2].[N+:19]([O-])([OH:21])=[O:20]>>[C:1]([NH:4][C:5]1[C:14]([N+:19]([O-:21])=[O:20])=[C:13]([C:15]([F:16])([F:17])[F:18])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:3])[CH3:2]

Komponenten

3

Edukt 2

HCID 944Nitric AcidHCID 11701649Methyl 2-(acetylamino)-4-(trifluoromethyl)benzoate

Produkt 1

HCID 67272857HCID 67272857, VerbindungAusbeute 38 %

Versuchsvorschrift

To an ice-cooled nitric acid (fuming) (20 ml) was added methyl 2-(acetylamino)-4-(trifluoromethyl)benzoate (7.30 g, 0.028 mol) portionwise and stirred for 30 min. The reaction mixture was poured into ice-water and extracted with ethyl acetate. The extracts were washed with aqueous saturated sodium bicarbonate and water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel with a 30% ethyl acetate/n-hexane to give 3.20 g (0.010 mol, 38%) of the title compound as a yellow powder.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe extracts were washed with aqueous saturated sodium bicarbonate and water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel with a 30% ethyl acetate/n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-8c60b5af2a6e4e2f820cfc7e37d26834
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08163935B2

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