関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyl-2-butanol | HCID 6405 | — |
| 反応物 | 1-Bromoheptane | HCID 12369 | — |
| 反応物 | Phenylboronic Acid | HCID 66827 | — |
| 反応物 | Di-tert-butyl(methyl)phosphanium tetraphenylborate(1-) | HCID 23136641 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 生成物 | Heptylbenzene | HCID 14115 | 89.1% |
反応手順
A 50-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 0.896 g (5 mmol) of n-heptyl bromide, 0.914 g (7.5 mmol) of phenylboronic acid, 0.056 g (0.25 mmol) of palladium (II) acetate, 1.683 g (15 mmol) of potassium tert-butoxide and 25 ml of tert-amyl alcohol were weighed in the flask, followed by stirring. Further, 0.240 g (0.5 mmol) of di-tert-butylmethylphosphonium tetraphenylborate obtained in Example B-1 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 25° C. for 24 hours. After the completion of the reaction, 20 ml of saturated sodium chloride solution was added, followed by separation. The organic phase was purified by column chromatography to afford 0.785 g of 1-phenylheptane (yield: 89 mol % based on n-heptyl bromide). The identification of the product was made by mass spectroscopy.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08124809B2 |
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| 出典データセット | uspto-grants-2012_02 |
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| ORD ID | ord-2e2d0db01e774cce85bfef4ec6c5ac44 |
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| 出典メモ | uspto-grants-2012_02 |
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