Ethanethiol → 3-Ethylthio-2-oxoglutaric acid

HRID 329538

Reaktionsgleichung

Reaktionsgleichung von HRID 329538
Br[CH:2]([CH2:8][C:9]([OH:11])=[O:10])[C:3](=[O:7])[C:4]([OH:6])=[O:5].[CH2:12]([SH:14])[CH3:13].C(N(CC)CC)C>ClCCl>[CH2:12]([S:14][CH:2]([CH2:8][C:9]([OH:11])=[O:10])[C:3](=[O:7])[C:4]([OH:6])=[O:5])[CH3:13]

Komponenten

5

Edukt 3

HCID 6343EthanethiolHCID 8471TriethylamineHCID 1959343-Bromo-2-ketoglutarate

Produkt 1

HCID 150978133-Ethylthio-2-oxoglutaric acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a suspension of 1.00 g of 3-bromo-2-oxoglutaric acid in 20 ml of dichloromethane was added 0.33 ml of ethane thiol while stirring under ice-cooling, followed by addition of 1.83 ml of triehtylamine. The reaction mixture was stirred at room temperature for 3 hours, then the solvent was distilled off. The residue was distributed to ethyl acetate and 1N-HCl. The ethyl acetate layer was separated, washed with water and dried (Na2SO4), followed by distilling off the solvent to give 0.82 g of 3-ethylthio-2-oxoglutaric acid as a pale yellow oily substance.

Aufarbeitung

  1. temperaturecooling
  2. stirringThe reaction mixture was stirred at room temperature for 3 hours
  3. distillationthe solvent was distilled off
  4. customThe ethyl acetate layer was separated
  5. washwashed with water
  6. dry with materialdried (Na2SO4)
  7. distillationby distilling off the solvent

Quellen und Nachweise

ORD-Eintrag
ord-75cd2c8c08a046d6bf2703cb55ebe0f2
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04891427

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