Sodium Formate → HCID 11830128, Verbindung

HRID 1654181

Reaktionsgleichung

Reaktionsgleichung von HRID 1654181
Br[CH:2]([CH3:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[F:12])=[O:4].C([O-])=[O:15].[Na+]>CO>[F:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[C:3](=[O:4])[CH:2]([OH:15])[CH3:13]

Komponenten

4

Edukt 2

HCID 2723810Sodium FormateHCID 110758302-Bromo-1-(2,4-difluorophenyl)propan-1-one

Produkt 1

HCID 11830128HCID 11830128, VerbindungAusbeute 47,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

2-Bromo-2',4'-difluoropropiophenone (141 g) was dissolved in methanol (1100 ml), to which was added sodium formate (176.2 g), and the mixture was stirred for 2 days at 50° C. Methanol was distilled off under reduced pressure. The residue was subjected to extraction by the addition of ethyl acetate (700 ml) and water (500 ml). The ethyl acetate layer was dried over magnesium sulfate, then the solvent was distilled off under reduced pressure. The residue was crystallized from hexane (200 ml) to afford 2',4'-difluoro-2-hydroxypropiophenone (50.5 g) as colorless prisms, m.p. 49°-51° C.

Aufarbeitung

  1. distillationMethanol was distilled off under reduced pressure
  2. extractionThe residue was subjected to extraction by the addition of ethyl acetate (700 ml) and water (500 ml)
  3. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was crystallized from hexane (200 ml)

Quellen und Nachweise

ORD-Eintrag
ord-e423fc196af7458b83ca05fe6d3ebaca
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05405861

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