참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 3-Methylcyclohexyl chloroformate | HCID 12705463 | — |
| 반응물 | N1-[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide | HCID 22866848 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 54231516 | HCID 54231516 | 79.5% |
반응 단계
0.4 g of N-methylmorpholine, and subsequently 0.8 g of 3-methylcyclohexyl chloroformate were added to a suspension containing 1.0 g of N1 -[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide suspended in 50 ml of methylene chloride at -15° C. The mixture was allowed to sit and warm naturally to room temperature and 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 then the methylene chloride was removed under reduced pressure. The residue was purified by column chromatography on silica gel, thus obtaining 1.2 g of the desired product in the form of a white crystal (yield: 80% ).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05574064 |
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| 출처 데이터셋 | uspto-grants-1996_11 |
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| ORD ID | ord-79bb7633d08d424ba82796a3a8d2600e |
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| 출처 메모 | uspto-grants-1996_11 |
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