2,3-Dihydroxybenzoic Acid → Ethyl 2,3-dihydroxybenzoate

HRID 565198

Reaktionsgleichung

Reaktionsgleichung von HRID 565198
[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.[CH2:17](O)[CH3:18]>>[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH2:17][CH3:18])=[O:5]

Komponenten

4

Edukt 3

HCID 192,3-Dihydroxybenzoic AcidHCID 702EthanolHCID 1118Sulfuric Acid

Produkt 1

HCID 2779843Ethyl 2,3-dihydroxybenzoateAusbeute 85 %

Versuchsvorschrift

A mixture of 2,3-dihydroxybenzoic acid(994 g), ethanol (3.8 L) and sulfuric acid (320 g) was refluxed for 44 hours. A portion of the solvent distilled out of the solution, and the solution was cooled and stirred overnight, and then further cooled in an ice/water bath. To the solution was added water (5.6 L). The solution was aged, and the crystals were filtered, washed with water, and dried to give ethyl 2,3-dihydroxybenzoate (1002 g, 85%); m.p. 66.0-67.2° C.

Aufarbeitung

  1. temperaturewas refluxed for 44 hours
  2. distillationA portion of the solvent distilled out of the solution
  3. temperaturethe solution was cooled
  4. temperaturefurther cooled in an ice/water bath
  5. additionTo the solution was added water (5.6 L)
  6. filtrationthe crystals were filtered
  7. washwashed with water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-532a442dbe104eeaad20cd38b10f718b
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06172062B2

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