関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,5-Difluorobenzonitrile | HCID 587204 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3,5-Difluorobenzylamine | HCID 145211 | — |
反応手順
A mixture of 3,5-difluorobenzonitrile (13.9 g., 0.10 mole) in methanol [(140 ml.), saturated with ammonia]and Raney nickel was shaken under hydrogen (50 psi.) for 1.5 hours and the solution was decanted from the catalyst. The solution was filtered, evaporated to an oil, and dissolved in ethyl acetate. The ethyl acetate solution was extracted twice with 1N HCl (75 ml.) and the aqueous solution was washed once with ethyl acetate, made basic with 10% sodium hydroxide, and extracted with three portions of ethyl acetate (100 ml.). The ethyl acetate solution was washed with water and brine, dried, and the solvent removed under vacuum. The residue was diluted with ether, filtered, and the solvent was removed under vacuum to give 3,5-difluorobenzylamine as an oil (11.7 g., 82%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04761415 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-0d11a5a0ac9547fa97c644a1d78afa6d |
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| 出典メモ | uspto-grants-1988_08 |
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