Methanol → Methyl 2,3,4-trimethoxybenzoate

HRID 1057946

Reaktionsgleichung

Reaktionsgleichung von HRID 1057946
[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[C:10]([O:14][CH3:15])[CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:21]O>>[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[C:10]([O:14][CH3:15])[CH:9]=[CH:8][C:4]=1[C:5]([O:7][CH3:21])=[O:6]

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 113082,3,4-Trimethoxybenzoic acid

Produkt 1

HCID 13940801Methyl 2,3,4-trimethoxybenzoate

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

2,3,4-trimethoxybenzoic acid (7.3 g) was dissolved in methanol (73 ml), mixed with sulfuric acid (15 ml), and stirred for 3 hours while heating at 80° C. The resultant was allowed to stand for cooling, evaporated under reduced pressure for removing the solvent, and the residue was added to cold water, followed by extraction with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate water and then with a saturated aqueous sodium chloride solution, dried over sodium sulfate anhydride, and evaporated under reduced pressure for removing the solvent to give Compound IIbt-a (6.8 g, 87%) as a colorless oily substance.

Aufarbeitung

  1. temperaturefor cooling
  2. customevaporated under reduced pressure
  3. customfor removing the solvent
  4. additionthe residue was added to cold water
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe organic layer was washed with saturated sodium bicarbonate water
  7. dry with materialwith a saturated aqueous sodium chloride solution, dried over sodium sulfate anhydride
  8. customevaporated under reduced pressure
  9. customfor removing the solvent
  10. customto give Compound IIbt-a (6.8 g, 87%) as a colorless oily substance

Quellen und Nachweise

ORD-Eintrag
ord-02da7c6493834e3c8659638193a9176f
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06514996B2

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