Methanol → HCID 57749798, Verbindung

HRID 553780Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 553780
[F:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([I:14])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].O=S(Cl)Cl.[CH3:19]O>>[CH3:19][O:5][C:4](=[O:6])[C:3]1[CH:7]=[C:8]([I:14])[CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:2]=1[F:1]

Komponenten

4

Edukt 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 57749803HCID 57749803, Verbindung

Produkt 1

HCID 57749798HCID 57749798, VerbindungAusbeute 96 %

Versuchsvorschrift

2-Fluoro-5-iodo-3-nitro-benzoic acid (2.0 g, 6.43 mmol) and SOCl2 (918 mg, 7.72 mmol) were added to 20 mL MeOH, and the mixture was refluxed for two hours and then cooled to room temperature. Solvent was evaporated under reduced pressure and the residue was dissolved in EtOAa. The EtOAc solution was washed with brine, dried over NaSO4, filtered and concentrated under reduced pressure to give 2.0 g (96%) of 2-fluoro-5-iodo-3-nitro-benzoic acid methyl ester.

Aufarbeitung

  1. temperaturethe mixture was refluxed for two hours
  2. customSolvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in EtOAa
  4. washThe EtOAc solution was washed with brine
  5. dry with materialdried over NaSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2d17a5eac188416fb8a9d27cfd3c4d9e
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08048905B2

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