関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Phenyl-1-propanone | HCID 7148 | — |
| 反応物 | Bromobenzene | HCID 7961 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Tri-tert-butylphosphonium tetra-para-tolylborate | HCID 23136639 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,2-Diphenylpropan-1-one | HCID 238518 | 98% |
反応手順
A 30-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 0.011 g (0.05 mmol) of palladium (II) acetate, 1.442 g (15 mmol) of sodium-tert-butoxide and 10 ml of tetrahydrofuran were weighed in the flask, followed by stirring. Further, 0.029 g (0.05 mmol) of tri-tert-butylphosphonium tetra-para-tolylborate obtained in Example B-3 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 25° C. for 30 minutes. 1.570 g (10 mmol) of bromobenzene was added, followed by stirring at 25° C. for 30 minutes. 1.476 g (11 mmol) of propiophenone was added, followed by stirring at 25° C. for 17 hours. After the completion of the reaction, 5 ml of water was added, followed by separation. The organic phase was purified by column chromatography to afford 2.061 g of 1,2-diphenyl-1-propanone (yield: 98 mol % based on bromobenzene). The identification of the product was made by mass spectroscopy, 1H-NMR and 13C-NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728176B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-95e39380ae354ac0977ad604490c471f |
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| 出典メモ | uspto-grants-2010_06 |
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