Reaktionsgleichung
[C:1]1([C:7]2[NH:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])([O-])=O.[K+].[K+].[Cl:22][CH2:23][CH2:24][CH2:25][CH2:26]I.O>CN(C)C=O>[Cl:22][CH2:23][CH2:24][CH2:25][CH2:26][N:11]1[C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[N:8]=[C:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2.5 g (12.88 mmol) of 2-phenyl-benzimidazole was dissolved in 30 ml of N,N-dimethylformamide, and 5.3 g (38.6 mmol) of K2CO3 and 2.0 ml (16.7 mmol) of 1-chloro-4-iodobutane were added to the resulting solution, followed by mixing the mixture at a room temperature for 10 hours. The reactant was combined with 100 ml of water and extracted with ethylacetate (70 ml×5) being washed with water and a sodium hydroxide solution, and then the combined organic layer was dried over anhydrous sodium sulfate and filtered. The solvent was removed from the filtrate under a reduced pressure, and the resulting residue was refined by silica gel column chromatography (n-hexane/ethylacetate=2/1) to obtain 3.5 g (yield 96%) of the title compound.
Aufarbeitung
- additionby mixing the mixture at a room temperature for 10 hours
- extractionextracted with ethylacetate (70 ml×5)
- washbeing washed with water
- dry with materiala sodium hydroxide solution, and then the combined organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- customThe solvent was removed from the filtrate under a reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-bcb62fb3cf794486aa6c3d206bc9a82f
- Quelldatensatz
- uspto-grants-2012_06
- Patentnummer
- US08198307B2
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