Acetic Acid → alpha-(2-fluorophenyl)-N-t-butylnitrone

HRID 636721

Reaktionsgleichung

Reaktionsgleichung von HRID 636721
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[CH3:10][C:11]([N+:14]([O-])=[O:15])([CH3:13])[CH3:12].C(O)(=O)C>C(O)C.[Zn]>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[N+:14]([C:11]([CH3:13])([CH3:12])[CH3:10])[O-:15]

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 116722-Methyl-2-nitropropaneHCID 67970o-Fluorobenzaldehyde

Produkt 1

HCID 85599391alpha-(2-fluorophenyl)-N-t-butylnitrone

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

To a suspension of 2-fluorobenzaldehyde (332.3 mg, 2.68 mmol), 1,1-dimethylnitroethane (547.5 mg, 5.31 mmol) and zinc (514.6 mg, 7.87 mmol) in ethanol (3.0 ml) was added acetic acid (940.2 mg, 15.7 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for 6.5 hours. Zinc acetate in the mixture was filtered off and the filtrate was concentrated and purified by silica gel chromatography (hexane/ethyl acetate=4/1 to 2/1).

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 6.5 hours
  2. filtrationZinc acetate in the mixture was filtered off
  3. concentrationthe filtrate was concentrated
  4. custompurified by silica gel chromatography (hexane/ethyl acetate=4/1 to 2/1)

Quellen und Nachweise

ORD-Eintrag
ord-61d658cb9eb749bda8fe13737e290f2a
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06194461B1

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