Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Chloroacetic Acid | HCID 300 | — |
| Edukt | 10-Methoxyiminostilbene | HCID 78424 | — |
| Edukt | Sodium Cyanate | HCID 517096 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | Oxcarbazepine | HCID 34312 | 24,8% |
Reaktionsschritte
A mixture of 100 gms of 10-methoxyiminostilbene in 1000 mL of toluene containing 106 gms of monochloro-acetic acid and 73 gms of sodium cyanate were heated to 40° C. under stirring and maintained for 4 hours. After completion of the reaction (monitored by HPLC and/or TLC), the mixture was cooled to room temperature, filtered and washed with 5% sodium carbonate solution followed by water. The toluene layer was then added to 1000 mL of 2N hydrochloric acid, and the mixture was heated to 75-80° C. and maintained for 2 hours under good agitation. It was then cooled to 0-5° C. and maintained for 2 hours, and the product oxcarbazepine was separated by filtration. This was then purified twice in toluene:methanol followed by methanol:dichloromethane solvent mixture to furnish 28 gms of pure oxcarbazepine.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06670472B2 |
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| Quelldatensatz | uspto-grants-2003_12 |
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| ORD ID | ord-f354caec36ad47a2a20c079ab1ea1e5d |
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| Quellennotiz | uspto-grants-2003_12 |
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