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-(4-tolyl)-N-phenylamino]acenaphthene | HCID 19688913 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-[N-(4-formylphenyl)-N-(4-tolyl)amino]acenaphthene | HCID 19688918 | 97.1% |
反応手順
4.7 g (0.014 mol) of the above prepared 5-[N-(4-tolyl)-N-phenylamino]acenaphthene was dissolved in 30 ml of N,N-dimethylformamide, and 3.22 g (0.021 mol) of phosphorus oxychloride was dropwise added thereto at room temperature for 10 minutes. After the temperature was raised to 50° C., and the mixture was stirred for 14 hours. The reaction was determined to be finished when disappearance of 5-[N-(4-tolyl)-N-phenylamino]acenaphthene was identified. The reaction product was poured into an aqueous solution having 10 g (0.23 mol) of 93% sodium hydroxide dissolved in 250 ml of water. The resultant mixture was cooled to precipitate a crystal, which was then filtrated, washed with water and dried to obtain 4.94 g (yield: 97.1%) of 5-[N-(4-formylphenyl)-N-(4-tolyl)amino]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-20078ac392344345839361b7b292e056 |
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| 出典メモ | uspto-grants-1998_03 |
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