참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 3-Methoxyphenyl carbonochloridate | HCID 22019180 | — |
| 반응물 | N1-[2-(4-cyanophenoxy)-1-methylethyl]L-valinamide hydrochloride | HCID 22866849 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N1-[2-(4-cyanophenoxy)-1-methylethyl]-N2-phenoxycarbonyl-L-valinamide | HCID 53713420 | 13.1% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05811424 |
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| 출처 데이터셋 | uspto-grants-1998_09 |
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| ORD ID | ord-a8975b2b51594056ad5e9bacda32a3b1 |
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| 출처 메모 | uspto-grants-1998_09 |
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