Methanol → Methyl 2',4'-difluoro-4-hydroxy-[1,1'-biphenyl]-3-carboxylate

HRID 1259013Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1259013
OS(O)(=O)=O.[CH:6]1[C:11]([C:12]2[CH:13]=[CH:14][C:15]([F:19])=[CH:16][C:17]=2[F:18])=[CH:10][C:9]([C:20]([OH:22])=[O:21])=[C:8]([OH:23])[CH:7]=1.[CH3:24]O>>[F:18][C:17]1[CH:16]=[C:15]([F:19])[CH:14]=[CH:13][C:12]=1[C:11]1[CH:6]=[CH:7][C:8]([OH:23])=[C:9]([C:20]([O:22][CH3:24])=[O:21])[CH:10]=1

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 3059Diflunisal

Produkt 1

HCID 491921Methyl 2',4'-difluoro-4-hydroxy-[1,1'-biphenyl]-3-carboxylateAusbeute 85 %

Versuchsvorschrift

H2SO4 (9.6 mL, 179.12 mmol) was added to a solution of diflunisal (15.0 g, 59.95 mmol) in MeOH (200 mL). The reaction mixture was refluxed for 12 h and it was allowed to reach r.t. Solids were collected by filtration and washed with cold MeOH (20 mL) to furnish 13.42 g of methyl 2′,4′-difluoro-4-hydroxybiphenyl-3-carboxylate (white solid, yield: 85%).

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 12 h
  2. customto reach r.t
  3. filtrationSolids were collected by filtration
  4. washwashed with cold MeOH (20 mL)

Quellen und Nachweise

ORD-Eintrag
ord-8c372d6800584a959ccff60b0a464fa9
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08466197B2

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