참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chloroacetic Acid | HCID 300 | — |
| 반응물 | 10-Methoxyiminostilbene | HCID 78424 | — |
| 반응물 | Sodium Cyanate | HCID 517096 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Oxcarbazepine | HCID 34312 | 24.8% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06670472B2 |
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| 출처 데이터셋 | uspto-grants-2003_12 |
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| ORD ID | ord-f354caec36ad47a2a20c079ab1ea1e5d |
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| 출처 메모 | uspto-grants-2003_12 |
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