Ethanethiol → 3-Ethylthio-2-oxoglutaric acid

HRID 1032034

Reaktionsgleichung

Reaktionsgleichung von HRID 1032034
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-5112f01feebd41dbbb44b92546e86d58
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04956358

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