Methanol → Methyl 2-hydroxy-6-methoxybenzoate

HRID 2117237

Reaktionsgleichung

Reaktionsgleichung von HRID 2117237
[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-29f75c0222e14271b3c012ee379abcbf
Quelldatensatz
uspto-grants-2008_10
Patentnummer
USRE040558E1

Verknüpfte Notizen

Wird geladen…