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 | 3-Methoxyphenyl carbonochloridate | HCID 22019180 | — |
| 反応物 | N1-[2-(4-cyanophenoxy)-1-methylethyl]L-valinamide hydrochloride | HCID 22866849 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N1-[2-(4-cyanophenoxy)-1-methylethyl]-N2-phenoxycarbonyl-L-valinamide | HCID 53713420 | 13.1% |
反応手順
1.0 g of N-methylmorpholine was added to a solution containing 1.5 g of N1 -[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide hydrochloride dissolved in 100 ml of methylene chloride, at -20° C. After 0.9 g of 3-methoxyphenyl chloroformate was added to the mixture at -20° C., the reaction mixture was allowed to sit and warm naturally to room temperature while being stirred. The whole mixture was stirred for 2 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 0.25 g of the desired product in the form of a white plated crystal (yield: 12%).
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-a8975b2b51594056ad5e9bacda32a3b1 |
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| 出典メモ | uspto-grants-1998_09 |
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