Methanol → Methyl 3,4-difluoro-2-hydroxybenzoate

HRID 577985

Reaktionsgleichung

Reaktionsgleichung von HRID 577985
[F:1][C:2]1[C:3]([OH:12])=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:18]O>O>[F:1][C:2]1[C:3]([OH:12])=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([O:7][CH3:18])=[O:6]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27582863,4-Difluoro-2-hydroxybenzoic acid

Produkt 1

HCID 46311128Methyl 3,4-difluoro-2-hydroxybenzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 3,4-difluoro-2-hydroxybenzoic acid (6.45 g, 37.05 mmol) and sulfuric acid (6 ml, 113 mmol) in MeOH (25 ml) was heated at reflux overnight. The mixture was diluted with water and extracted with ether. The ether was washed with aqueous NaHCO3, water and brine. The combined aqueous layers were twice more extracted with ether, which was washed with NaHCO3, water, and brine. The combined ether extracts were dried (MgSO4) and concentrated to give 6.4 g of product as a white solid.

Aufarbeitung

  1. temperatureat reflux overnight
  2. extractionextracted with ether
  3. washThe ether was washed with aqueous NaHCO3, water and brine
  4. extractionThe combined aqueous layers were twice more extracted with ether, which
  5. washwas washed with NaHCO3, water, and brine
  6. dry with materialThe combined ether extracts were dried (MgSO4)
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-dc05634c906247dc8ab09044c6c4c294
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09040528B2

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