참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanolamine | HCID 700 | — |
| 반응물 | Nicotinate | HCID 937 | — |
| 반응물 | N-hydroxysuccinamide | HCID 18381240 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-(2-hydroxyethyl)nicotinamide | HCID 72663 | 73% |
반응 단계
The ethanolamine was dissolved in dried N,N-di-methyl formamide (DMF) and chilled in an ice bath. The nicotinate derivative, also dissolved in DMF, was added to the DMF-amine mixture, dropwise under a nitrogen atmosphere. As the nicotinate derivative was added, the mixture turned milky and was slurried for at least one half hour. The milky substance was the N-hydroxy-succinamide precipitating, which was filtered off. The DMF-mixture was washed with ether to remove any precipitant. The solvent mixture was removed under high vaccum. The oily residue was triturated with ether, yielding a precipitant, N-(2-hydroxyethyl)-nicotinamide, which was recrystallized from ethyl acetate/petroleum ether. This compound had a melting point of 86°-87° C.; and Rf value of 0.30 (TLC: silica: chloroform/methanol (10:1)); and a yield of 73%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04764462 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-7f0b6dc3b4ec4a73b4593ba147c30853 |
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| 출처 메모 | uspto-grants-1988_08 |
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