Carbonic acid-guanidine (1:1) → HCID 178468831, 화합물

HRID 2387797노트

반응식

HRID 2387797 반응식
[C:1](=O)(O)O.[NH2:5][C:6]([NH2:8])=[NH:7].[CH3:9][O:10][C:11](=[O:28])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][CH:19]([C:23](OCC)=[O:24])[C:20](=O)[CH3:21])[CH:13]=1>CCO>[CH2:9]([O:10][C:11](=[O:28])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][C:19]2[C:23]([OH:24])=[N:7][C:6]([NH2:8])=[N:5][C:20]=2[CH3:21])[CH:13]=1)[CH3:1]

참가 물질

4

반응물 2

HCID 286947Carbonic acid-guanidine (1:1)HCID 23005490HCID 23005490, 화합물

생성물 1

HCID 178468831HCID 178468831, 화합물수율 96.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Guanidine carbonate (2.71 g) was added to a stirred solution of 3-(2-ethoxycarbonyl-3-oxobutyl)-benzoic acid methyl ester (2.12 g) in EtOH (40 mL). The reaction mixture was heated to reflux for 6 h and allowed to cool. The solvent was evaporated under reduced pressure and the residue suspended in water (30 mL). The resulting precipitate was collected by filtration and the solid suspended in EtOAc (30 mL). The solid was collected by filtration to give the subtitle compound as a colourless solid 2.12 g that was used without further purification.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 6 h
  3. temperatureto cool
  4. customThe solvent was evaporated under reduced pressure
  5. filtrationThe resulting precipitate was collected by filtration
  6. filtrationThe solid was collected by filtration

출처 및 근거

ORD 기록
ord-e8372107c8424546b5ce029fae8c58d5
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268990B2

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