Reaktionsgleichung
[C:1]([C:6]1[N:10]([CH3:11])[C:9]([S:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[N:8][C:7]=1[CH3:22])(OCC)=[O:2].[H-].[Al+3].[H-].[H-].[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[OH-].[Na+]>CCOCC.O>[CH3:11][N:10]1[C:6]([CH2:1][OH:2])=[C:7]([CH3:22])[N:8]=[C:9]1[S:12][CH2:13][C:14]1[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=1Komponenten
8
Edukt 5
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
5-Carbethoxy-1,4-dimethyl-2-(4-methoxybenzylthio)imidazole (31 g, 0.1 mole) dissolved in ether (250 ml) was added dropwise to a solution of aluminum hydride in ether stirred at 0° C. [the aluminum hydride in ether was prepared by adding lithium aluminum hydride (7.4 g, 0.19 mole) in portions to a solution of aluminum chloride (8.6 g, 0.065 mole) stirred in ether (200 ml) at 0° C⟧ The mixture was stirred at 0° C. for 1 hour, treated with water and 10% aqueous sodium hydroxide, filtered and concentrated in vacuo. The resulting oil was dissolved in methylene chloride, dried with magnesium sulfate, filtered and concentrated in vacuo to give 1,4-dimethyl-5-hydroxymethyl-2-(4-methoxybenzylthio)imidazole.
Aufarbeitung
- customwas prepared
- filtrationfiltered
- concentrationconcentrated in vacuo
- dissolutionThe resulting oil was dissolved in methylene chloride
- dry with materialdried with magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-6a7dc7cd8ded4a3c9867fe85a2edfb94
- Quelldatensatz
- uspto-grants-1988_09
- Patentnummer
- US04769386
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