Ethanethiol → 3-Ethylthio-2-oxoglutaric acid

HRID 329538

反応式

HRID 329538 の反応式
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

反応物 3

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

生成物 1

HCID 150978133-Ethylthio-2-oxoglutaric acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

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

  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

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

関連ノート

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