Carbonic acid-guanidine (1:1) → HCID 178497677, Verbindung

HRID 1617160Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1617160
C(=O)(O)O.[NH2:5][C:6]([NH2:8])=[NH:7].C([O:11][C:12]([CH:14]([C:27](=O)[CH3:28])[CH2:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][C:17]=1[F:26])=O)C>CO>[NH2:7][C:6]1[N:8]=[C:12]([OH:11])[C:14]([CH2:15][C:16]2[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][C:17]=2[F:26])=[C:27]([CH3:28])[N:5]=1

Komponenten

4

Edukt 2

HCID 286947Carbonic acid-guanidine (1:1)HCID 68412608Methyl 4-(2-(ethoxycarbonyl)-3-oxobutyl)-3-fluorobenzoate

Produkt 1

HCID 178497677HCID 178497677, VerbindungAusbeute 60,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Guanidine carbonate (6.86 g) was added to a stirred solution of the product from step (i) (11.1 g) in MeOH (200 mL). The resulting mixture was stirred at 70° C. for 15 h. The mixture was allowed to cool to rt and the resulting precipitate collected by filtration. The solid was suspended in water (50 mL), collected by filtration and washed with MeOH to give the subtitle compound as a colourless solid 6.60 g that was used without further purification.

Aufarbeitung

  1. temperatureto cool to rt
  2. filtrationthe resulting precipitate collected by filtration
  3. filtrationcollected by filtration
  4. washwashed with MeOH

Quellen und Nachweise

ORD-Eintrag
ord-66d9c34f951b424ebc17433fa66c3697
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08765939B2

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