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Ethylamine → Ethyl (ethylamino)(oxo)acetate

HRID 2408466
ノート
印刷プレビュー

反応式

HRID 2408466 の反応式
C(O[C:4](=[O:10])[C:5]([O:7][CH2:8][CH3:9])=[O:6])C.[CH2:11]([NH2:13])[CH3:12]>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].ClCCl.O>[CH2:8]([O:7][C:5](=[O:6])[C:4]([NH:13][CH2:11][CH3:12])=[O:10])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 6341EthylamineHCID 7268Diethyl Oxalate

生成物 1

HCID 3413435Ethyl (ethylamino)(oxo)acetate収率 41.3%

試薬・触媒・溶媒 3

HCID 21218Trioctylmethylammonium chloride触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To 135,8 ml (1000 mM) of diethyloxalate and 1 g of aliquat 336, in 1000 ml of dichloromethane, were added 64 ml (1000 mM) of ethylamine at 70% in water. The reaction mixture was stirred at room temperature for 72 h. The reaction mixture was dried over anhydrous sodium sulfate and the solvent was removed under vacuum to give an oil, which was further purified by silica gel column chromatography, using dichloromethane/dimethylketone (95/5) as eluant, to give 59.9 g of ethyl(ethyl amino)(oxo)acetate as an oil.

後処理

  1. dry with materialThe reaction mixture was dried over anhydrous sodium sulfate
  2. customthe solvent was removed under vacuum
  3. customto give an oil, which
  4. customwas further purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e47a50fc6abd494a8d53261589d26157
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08815859B2

反応ノート

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