참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Beta-Alanine | HCID 239 | — |
| 반응물 | Benzaldehyde | HCID 240 | — |
| 반응물 | 4-methyl-3-oxo-N-phenylpentanamide | HCID 10219899 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Benzylidene-4-methyl-3-oxo-N-phenylpentanamide | HCID 53394866 | 84.7% |
반응 단계
A suspension of 100 kg of 4-methyl-3-oxo-N-phenyl-pentanamide (Example B) in 660 kg of hexanes is treated with agitation under nitrogen with 8 kg of β-alanine, 47 kg of benzaldehyde, and 13 kg of glacial acetic acid. The resulting suspension is heated to reflux with removal of water for 20 hours. An additional 396 kg of hexanes and 3 kg of glacial acetic acid is added and reflux continued with water removal for one hour. The reaction mixture is cooled to 20°-25° C. and the product is isolated by filtration. The product is purified by slurrying in hexanes at 50°-60° C., cooling, and filtration. The product is slurried twice with water at 20°-25° C., filtered, and dried in vacuo to yield 110 kg of 4-methyl-3-oxo-N-phenyl-2-(phenylmethylene)pentanamide, mp 143.7°-154.4° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05245047 |
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| 출처 데이터셋 | uspto-grants-1993_09 |
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| ORD ID | ord-37e8689612b643c69b9ba6881e96180a |
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| 출처 메모 | uspto-grants-1993_09 |
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