関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-(N,N-diphenylamino)acenaphthene | HCID 19688919 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-[N-(4-formylphenyl)-N-phenylamino]acenaphthene | HCID 19688917 | 86.6% |
反応手順
32.14 g (0.1 mol) of the above prepared 5-(N,N-diphenylamino)acenaphthene was dissolved in 300 ml of N,N-dimethylformamide, and 22.73 g (0.15 mol) of phosphorus oxychloride was dropwise added thereto at room temperature for 30 minutes. After raising the temperature to 50° C., the reaction mixture was stirred for 14 hours. The reaction was determined to be finished when disappearance of 5-(N,N-diphenylamino)acenaphthene was identified. The reaction product was poured into an aqueous solution having 45 g (1.05 mol) of 93% sodium hydroxide dissolved in 1000 ml of water. The resultant mixture was cooled to precipitate a crystal, and the crystal was filtrated, washed with water and dried to obtain 30.27 g (yield: 86.6%, melting point: 138.0°-141.0° C.) of 5-[N-(4-formylphenyl)-N-phenylamino]acenaphthene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728500 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-c9df1b4f59204cf6ba44f7f63a8372d9 |
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| 出典メモ | uspto-grants-1998_03 |
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