참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,5-Difluorobenzonitrile | HCID 587204 | — |
| 촉매 | Nickel | HCID 935 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3,5-Difluorobenzylamine | HCID 145211 | — |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04761415 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-0d11a5a0ac9547fa97c644a1d78afa6d |
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| 출처 메모 | uspto-grants-1988_08 |
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