関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 3,5-Bis(trifluoromethyl)benzonitrile | HCID 96746 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3,5-Bis(trifluoromethyl)benzylamine | HCID 521099 | 85.1% |
反応手順
At first, a 1-liter autoclave equipped with a mechanical stirrer was charged with 200 g (0.84 mol) of 3,5-bis(trifluoromethyl)benzonitrile, 200 ml of methanol, and 6 g of a catalyst (i.e., a carbon powder (50% wet) carrying thereon 5% palladium), followed by introduction of 14 g of liquid ammonia and then introduction of hydrogen to have a pressure of 1 MPa. Then, the reaction mixture was stirred, while the reaction temperature was maintained at 20° C. and while hydrogen was gradually introduced into the autoclave in a manner to maintain the total pressure at 1 MPa. After conducting the reaction for 3 hr, the reaction was stopped, followed by removing the catalyst by filtration. As a result of analyzing the obtained reaction liquid by gas chromatography, 3,5-bis(trifluoromethyl)benzylamine was formed at a yield of 85.1%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06362372B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-c1f621d96598450680a715430b72c700 |
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| 出典メモ | uspto-grants-2002_03 |
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