反应详情

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.

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