関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Anthraquinonecarboxylic acid | HCID 67030 | — |
| 反応物 | Diethyl cyanophosphonate | HCID 76257 | — |
| 反応物 | 4,5,6,7-Tetrahydrofuro[2,3-c]pyridine hydrochloride | HCID 19599907 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-(Anthraquinone-2-carbonyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine | HCID 19599963 | — |
反応手順
To a solution of 0.160 g (1.000 mmol) of 4,5,6,7-tetrahydrofuro[2,3-c]pyridine hydrochloride, 0.302 g (1.2 mmol) of anthraquinone-2-carboxylic acid and 0.55 ml (4.0 mmol) of triethylamine in 30 ml of dichloromethane, 0.24 g (1.5 mmol) of diethyl cyanophosphonate was added under ice-cooling, followed by overnight stirring at room temperature. The reaction mixture was poured into water and extracted with dichloromethane 2 times. The combined organic layer was washed with water and dried over anhydrous sodium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=3/1 to 2/1); the resulting solid was washed with ethyl acetate to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05998433 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-200035bc39454bcb9d92fd4df9cd3b4a |
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| 出典メモ | uspto-grants-1999_12 |
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