関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromophenylhydrazine hydrochloride | HCID 12157 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Phenylbenzylglyoxal | HCID 11096234 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(p-Bromophenyl)-3,5-diphenylpyrazole | HCID 4645096 | 68.8% |
反応手順
In a 500-ml four-necked flask were placed 25.2 g (0.11 mole) of 1,3-diphenylpropanedione, 25.3 g (0.11 mole) of p-bromophenylhydrazine hydrochloride, and 234.7 g of toluene. The mixture was stirred at room temperature and 6.0 g (0.11 mole) of sodium methoxide was added in drops at room temperature. After the addition, the mixture was heated under reflux with stirring for three hours. Upon completion of the reaction, the reaction mixture was cooled to room temperature and a solid was recovered by filtration. The filtrate was concentrated under reduced pressure to dryness. To the residue was added 350 ml of methanol and the mixture was heated with stirring for one hour. Thereafter, the mixture was cooled to room temperature and a solid was recovered by filtration. The solid was washed with methanol and dried under reduced pressure to give 28.4 g of 1-(p-bromophenyl)-3,5-diphenylpyrazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07816020B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-0d23d9d2ba29467f81878ea3554623ed |
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| 出典メモ | uspto-grants-2010_10 |
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