2,3-Dihydroxybenzoic Acid → Methyl 2,3-Dihydroxybenzoate

HRID 489141

Reaktionsgleichung

Reaktionsgleichung von HRID 489141
[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:17]O>>[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:17])=[O:5]

Komponenten

4

Versuchsvorschrift

A mixture of 2,3-dihydroxybenzoic acid (3.8 g, 24.6 mmol) in methanol (300 ml) was treated dropwise with conc. Sulfuric acid (4.2 g) and the resultant solution was heated at reflux temperature overnight. Upon cooling the solvent was evaporated and the residue poured into ice-water. The mixture was extracted with dichloromethane (3×50 ml) and the combined organic fractions dried (Na2SO4) and concentrated to yield a pale tan solid (4.05 g).

Aufarbeitung

  1. temperatureat reflux temperature overnight
  2. temperatureUpon cooling the solvent
  3. customwas evaporated
  4. additionthe residue poured into ice-water
  5. extractionThe mixture was extracted with dichloromethane (3×50 ml)
  6. dry with materialthe combined organic fractions dried (Na2SO4)
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-ee1b46de3f4c429aa2531db13f266d31
Quelldatensatz
uspto-grants-2005_12
Patentnummer
US06977255B2

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