Hydrochloric Acid → HCID 178488125, Verbindung
Reaktionsgleichung
[CH3:1][O:2][C:3]1[CH:22]=[CH:21][C:6]2[NH:7][C:8]([S:10][CH2:11][C:12]3[C:17]([CH3:18])=[C:16](Cl)[C:15]([CH3:20])=[CH:14][N:13]=3)=[N:9][C:5]=2[CH:4]=1.[CH3:23][OH:24].C[O-].[Na+].Cl>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:22]=[CH:21][C:6]2[NH:7][C:8]([S:10][CH2:11][C:12]3[C:17]([CH3:18])=[C:16]([O:24][CH3:23])[C:15]([CH3:20])=[CH:14][N:13]=3)=[N:9][C:5]=2[CH:4]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
First, 277 mg (0.92 mmol) of 5-methoxy-2-{[(4-chloro-3,5-dimethyl-2-pyridyl)methyl]thio}-1H-benzimidazole obtained in Example 21 and 1.00 g (5.20 mmol) of methanol 28% solution of sodium methoxide were introduced to a 3-necked flask (30 ml volume) equipped with a thermometer, a magnetic stirrer and a condenser tube, and the mixture was agitated for 10 hours while being slowly refluxed. Then the mixture was neutralized with dilute hydrochloric acid. Ethyl acetate (10 ml) was added thereto and an organic layer was separated, and an aqueous layer was extracted twice with 10 ml of ethyl acetate. The extracts and the above mentioned organic layer were combined and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give 232 mg of 5-methoxy-2-{[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]thio}-1H-benzimidazole (yield of 85%) with revealing the properties.
Aufarbeitung
- customequipped with a thermometer, a magnetic stirrer and a condenser tube
- temperaturewhile being slowly refluxed
- customan organic layer was separated
- extractionan aqueous layer was extracted twice with 10 ml of ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was removed under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-c7acea8fdad1486389d5ad137a571cc3
- Quelldatensatz
- uspto-grants-2001_03
- Patentnummer
- US06197962B1
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