Dimethylformamide → 4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-2-[1,2,4]triazol-1-yl-1H-benzimidazole
Reaktionsgleichung
[H-].[Na+].CN(C)C=O.[F:8][C:9]1[CH:35]=[CH:34][C:12]([O:13][C:14]2[C:22]3[N:21]=[C:20](S(C)(=O)=O)[NH:19][C:18]=3[CH:17]=[C:16]([O:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)[CH:15]=2)=[CH:11][CH:10]=1.[NH:36]1[CH:40]=[N:39][CH:38]=[N:37]1>C(OCC)(=O)C>[F:8][C:9]1[CH:35]=[CH:34][C:12]([O:13][C:14]2[C:22]3[N:21]=[C:20]([N:36]4[CH:40]=[N:39][CH:38]=[N:37]4)[NH:19][C:18]=3[CH:17]=[C:16]([O:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)[CH:15]=2)=[CH:11][CH:10]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 160 °C
Versuchsvorschrift
5.0 mg of sodium hydride was added to a dimethylformamide (0.5 ml) solution of 16 mg of 4-(4-fluoro-phenoxy)-2-methanesulfonyl-6-(pyridin-3-yloxy)-1H-benzimidazole, and then 10.4 mg of [1,2,4]triazole was added to it, and the reaction liquid was stirred overnight at 160° C. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate) to obtain the entitled compound.
Aufarbeitung
- customthe reaction liquid
- customThe reaction liquid
- washwashed with water and saturated saline in order
- dry with materialdried with anhydrous magnesium sulfate
- customThe solvent was evaporated away under reduced pressure
- customthe resulting residue was purified
- customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate)
- customto obtain the entitled compound
Quellen und Nachweise
- ORD-Eintrag
- ord-5739102b7b02496e84958cd0c1d66046
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07728025B2
Notizen zur Reaktion
Wird geladen…