Benzimidazole → 1H-Benzimidazole, 1-methyl-
Reaktionsgleichung
[CH3:1]I.[OH-].[K+].[N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][CH:6]=1>C(O)C.O>[CH3:1][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[N:7]=[CH:6]1Komponenten
6
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
14.1 g of methyl iodide and 6.15 g of potassium hydroxide were added to a suspension of 11.8 g of benzimidazole in 50 ml of ethanol and 30 ml of water and the mixture was refluxed for 6 hours and was then cooled. The mixture was extracted three times with chloroform and the combined chloroform extracts were dried and filtered. The filtrate was evaporated to dryness and the oily residue was chromatographed over neutral alumina. Elution with chloroform yielded 1-methyl-benzimidazole as a crude oil which was used as is for the next step.
Aufarbeitung
- temperaturethe mixture was refluxed for 6 hours
- temperaturewas then cooled
- extractionThe mixture was extracted three times with chloroform
- dry with materialthe combined chloroform extracts were dried
- filtrationfiltered
- customThe filtrate was evaporated to dryness
- customthe oily residue was chromatographed over neutral alumina
- washElution with chloroform
Quellen und Nachweise
- ORD-Eintrag
- ord-d0da4f3d7c0e4e4b8179c663b488848e
- Quelldatensatz
- uspto-grants-1979_04
- Patentnummer
- US04151280
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