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

HRID 2387797Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2387797
[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]

Komponenten

4

Edukt 2

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

Produkt 1

HCID 178468831HCID 178468831, VerbindungAusbeute 96,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-e8372107c8424546b5ce029fae8c58d5
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08268990B2

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