化工社化工社 化学情報印刷レポート · 研究参考用
Benzoic Acid → HCID 69996526、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic Acid | HCID 243 | — |
| 反応物 | 10-Methoxyiminostilbene | HCID 78424 | — |
| 反応物 | Sodium Cyanate | HCID 517096 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 69996526 | HCID 69996526 | — |
反応手順
An especially preferred method according to this invention comprises reaction of 10-methoxy-5H-dibenz[b,f]azepine with benzoic acid and sodium cyanate in toluene at reflux temperature to give 10-methoxy-5H-dibenz[b,f]azepine carboxamide as a major product (such as about 75%), along with 10-oxo-iminodibenzyl and other impurities. The reaction mixture is thereafter filtered and washed with water, and the toluene layer taken as such for hydrolysis in a biphasic system (aqueous hydrochloric acid/toluene) to furnish oxcarbazepine, which is purified just once (whereas twice at least is needed when the prior art process is carried out) in a mixture of methanol and dichloromethane (Scheme-5).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06670472B2 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-2e7260cd72704e56a2d7eece95a081ea |
| 出典メモ | uspto-grants-2003_12 |