Urea → (2,5-Dioxo-imidazolidin-4-ylidene)-ethoxy-acetic acid ethyl ester

HRID 628973ノート

反応式

HRID 628973 の反応式
[CH2:1]([O:3][CH:4]([C:10](=O)[C:11]([O:13]CC)=O)[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2].[NH2:17][C:18]([NH2:20])=[O:19].Cl.CC(O)=O>>[CH2:8]([O:7][C:5](=[O:6])[C:4](=[C:10]1[C:11](=[O:13])[NH:20][C:18](=[O:19])[NH:17]1)[O:3][CH2:1][CH3:2])[CH3:9]

参加物

4

反応物 3

HCID 1176UreaHCID 111389942-Ethoxy-3-oxo-succinic acid diethyl esterHCID 22641269Acetate-hydrochloric acid

生成物 1

HCID 67295487(2,5-Dioxo-imidazolidin-4-ylidene)-ethoxy-acetic acid ethyl ester

実験手順

A mixture of diethyl 2-ethoxy-3-oxo-succinate (55.86 g, 1 eq) and urea (14.41 g, 1 eq.) was refluxed for 2.5 h in 1 M HCl—AcOH (1200 ml, 5 eq.) and allowed to become cool. The cooled mixture was evaporated to dryness. The residues were dissolved in MeOH, heated aside for crystallization. After crystallization, the precipitates were filtered to give a product which was an off-white solid (15.11 g, 27.5%).

後処理

  1. temperatureto become cool
  2. customThe cooled mixture was evaporated to dryness
  3. dissolutionThe residues were dissolved in MeOH
  4. temperatureheated aside for crystallization
  5. customAfter crystallization
  6. filtrationthe precipitates were filtered
  7. customto give a product which

出典と根拠

ORDレコード
ord-1cfb294b25b94352b171941aab719456
出典データセット
uspto-grants-2016_04
特許番号
US09315491B2

反応ノート

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