Ammonium Chloride → HCID 66612181, Verbindung

HRID 2390470Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2390470
F[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]1[N:12]([CH3:13])[C:11]2[CH:14]=[CH:15][C:16]([C:18]([F:21])([F:20])[F:19])=[CH:17][C:10]=2[N:9]=1.[CH3:22][O-:23].[Na+].[Cl-].[NH4+]>CN(C=O)C>[CH3:22][O:23][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]1[N:12]([CH3:13])[C:11]2[CH:14]=[CH:15][C:16]([C:18]([F:21])([F:20])[F:19])=[CH:17][C:10]=2[N:9]=1

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 10942334Sodium MethoxideHCID 666115222-(3-fluoropyridin-4-yl)-1-methyl-5-trifluoromethyl-1H-benzimidazole

Produkt 1

HCID 66612181HCID 66612181, VerbindungAusbeute 89,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a mixture of 0.30 g of 2-(3-fluoropyridin-4-yl)-1-methyl-5-trifluoromethyl-1H-benzimidazole and 10 ml of DMF was added 0.16 g of sodium methoxide under ice cool, then, the mixture was heated up to room temperature and stirred for 1.5 hours. A saturated ammonium chloride aqueous solution was poured, and the mixture was extracted three times with ethyl acetate. The combined organic layers were dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.28 g of 2-(3-methoxypyridin-4-yl)-1-methyl-5-trifluoromethyl-1H-benzimidazole (hereinafter, referred to as present active compound 8).

Aufarbeitung

  1. temperaturecool
  2. extractionthe mixture was extracted three times with ethyl acetate
  3. dry with materialThe combined organic layers were dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c986f30220454f078321b81da531ab60
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08273764B2

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