Ethanethiol → 3-Ethylthio-2-oxoglutaric acid
反応式
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]参加物
5
実験手順
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.
後処理
- temperaturecooling
- stirringThe reaction mixture was stirred at room temperature for 3 hours
- distillationthe solvent was distilled off
- customThe ethyl acetate layer was separated
- washwashed with water
- dry with materialdried (Na2SO4)
- distillationby distilling off the solvent
出典と根拠
- ORDレコード
- ord-75cd2c8c08a046d6bf2703cb55ebe0f2
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04891427
反応ノート
読み込み中…