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

HRID 628973노트

반응식

HRID 628973 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-1cfb294b25b94352b171941aab719456
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315491B2

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