Methanol → HCID 86649400, Verbindung

HRID 80154

Reaktionsgleichung

Reaktionsgleichung von HRID 80154
[CH3:1][O:2][NH2:3].C([O-])([O-])=O.[K+].[K+].[F:10][C:11]1[CH:18]=[C:17]([N:19]2[CH2:23][CH2:22][N:21]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][C:29]=3[CH3:30])[C:20]2=[O:31])[CH:16]=[CH:15][C:12]=1[CH:13]=O.CO>C(COC)OC.C(Cl)(Cl)Cl>[CH3:1][O:2][N:3]=[CH:13][C:12]1[CH:15]=[CH:16][C:17]([N:19]2[CH2:23][CH2:22][N:21]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][C:29]=3[CH3:30])[C:20]2=[O:31])=[CH:18][C:11]=1[F:10]

Komponenten

7

Edukt 4

HCID 887MethanolHCID 4113O-MethylhydroxylamineHCID 11430Potassium CarbonateHCID 596361642-Fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde

Produkt 1

HCID 86649400HCID 86649400, VerbindungAusbeute 9,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

O-Methyl-hydroxylamine (84 mg, 1.003 mmol) and K2CO3 (207 mg, 1.5 mmol) were added to a solution of 2-fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde-(I-121a: 300 mg, 1.003 mmol) in dimethoxyethane (10 mL). The resulting mixture was heated to 40° C. for 2 hours. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was filtered, washed with CHCl3 and the filtrate was concentrated under reduced pressure to afford 30 mg of crude 2-Fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde O-methyl-oxime, which was used in the next step without further purification.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. washwashed with CHCl3
  3. concentrationthe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-faec1e1876794e68b942d7f8dbe08414
Quelldatensatz
uspto-grants-2014_09
Patentnummer
USRE045173E1

Verknüpfte Notizen

Wird geladen…