関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Phenyl thioxochloroformate | HCID 70498 | — |
| 反応物 | N1-[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide | HCID 22866848 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N1-[2-(4-cyanophenoxy)-1-methylethyl]-N2-phenoxycarbonyl-L-valinamide | HCID 53713420 | 76.7% |
反応手順
0.4 g of N-methylmorpholine was added to a suspension containing 1.1 g of N1 -[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide suspended in 40 ml of methylene chloride, at -15° C. After 0.7 g of phenyl chlorothionoformate was added to the mixture at -15° C., the reaction mixture was allowed to sit and warm naturally to room temperature while being stirred, and then the whole mixture was stirred for 15 hours at room temperature. Water was subsequently added to the reaction mixture. After the methylene chloride layer was washed with water, the organic layer was dried over anhydrous magnesium sulfate and the methylene chloride was removed under reduced pressure. The residue was purified by column chromatography on silica gel, thus yielding 1.2 g of the desired product in the form of a yellow glutinous substance (yield: 75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05811424 |
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| 出典データセット | uspto-grants-1998_09 |
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| ORD ID | ord-d3459f31632b4562aafcf48ee493a05f |
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| 出典メモ | uspto-grants-1998_09 |
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