Methanol → Methyl 2-hydroxy-6-methoxybenzoate

HRID 988284

Reaktionsgleichung

Reaktionsgleichung von HRID 988284
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([OH:12])[C:8]=1[C:9]([OH:11])=[O:10].[CH3:13]O>S(=O)(=O)(O)O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([OH:12])[C:8]=1[C:9]([O:11][CH3:13])=[O:10]

Komponenten

4

Edukt 2

HCID 887MethanolHCID 5915242-Hydroxy-6-methoxybenzoic acid

Produkt 1

HCID 527092Methyl 2-hydroxy-6-methoxybenzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

A mixture of 6-methoxysalicylic acid (10.0 g, 59.5 mmol) in methanol (40 mL) and sulfuric acid (2 mL) is heated at reflux 48 h. Although some acid remains the reaction is concentrated to remove the methanol and partitioned between ethyl acetate and saturated sodium carbonate solution. The organic phase is separated and washed with sodium carbonate until no acid remains by TLC analysis. The organic phase is dried and concentrated to provide the title compound as a low melting solid.

Aufarbeitung

  1. temperatureis heated
  2. temperatureat reflux 48 h
  3. concentrationis concentrated
  4. customto remove the methanol
  5. custompartitioned between ethyl acetate and saturated sodium carbonate solution
  6. customThe organic phase is separated
  7. washwashed with sodium carbonate until no acid
  8. customThe organic phase is dried
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-867682a462d647e6b382d695393bf0f8
Quelldatensatz
uspto-grants-2003_10
Patentnummer
US06635655B1

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