関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromobenzene | HCID 7961 | — |
| 反応物 | Diphenylamine | HCID 11487 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | n-Butyldicyclohexylphosphonium tetraphenylborate | HCID 23136652 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Triphenylamine | HCID 11775 | 85% |
反応手順
A 100-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 7.536 g (48 mmol) of bromobenzene, 6.769 g (40 mmol) of diphenylamine, 4.613 g (48 mmol) of sodium-tert-butoxide, 0.090 g (0.40 mmol) of palladium (II) acetate and 5 ml of xylene were weighed in the flask, followed by stirring. Further, 0.690 g (1.20 mmol) of n-butyldicyclohexylphosphonium tetraphenylborate obtained in Example B-47 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 125° C. for 4 hours. After the completion of the reaction, 45 ml of xylene and 50 ml of saturated sodium chloride solution were added, followed by separation. The organic phase was purified by column chromatography to afford 8.345 g of triphenylamine (yield: 85 mol % based on diphenylamine). The melting point was 125-126° C.
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-fc2edff262d145d48019701486a39b6c |
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| 出典メモ | uspto-grants-2010_06 |
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