関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Aminoterephthalic acid | HCID 2724822 | — |
| 溶媒 | Diphenyl Ether | HCID 7583 | — |
| 溶媒 | Cyclohexanone | HCID 7967 | — |
| 生成物 | 9-Oxo-5,6,7,8,9,10-hexahydro-acridine-3-carboxylic acid | HCID 57516453 | — |
反応手順
To a suspension of 2-amino terephthalic acid (12 g, 6.6 mmols) in diphenyl ether (120 mL), cyclohexanone (25 mL) was added and the reaction mixture was heated to 250° C. for 10 min. Reaction completion was monitored by LC/MS (75% starting material and 25% Product formation was observed). Cyclohexanone (25 mL) was added and the reaction mixture was heated to 250° C. for another 10 min. (LC/MS showed 50% product formation). The above process was repeated till LC/MS showed complete product formation (Starting material <2%). The reaction mixture was cooled to 25° C., product was filtered, washed with hexane (100 mL) and dried under vacuum to get 15.8 g of (Via) (98%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09328093B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-180e7a29ffa640f6a54e1a4090cba6a0 |
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| 出典メモ | uspto-grants-2016_05 |
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