참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | L-Valinol | HCID 640993 | — |
| 반응물 | 2-(2-Furanyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one | HCID 24739960 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-[[1-[(2-Furanylcarbonyl)amino]cyclohexyl]carbonyl]-L-valinol | HCID 24876087 | 74.7% |
반응 단계
A solution of 8.81 ml (50.6 mmol) of N,N-diisopropylethylamine and 2.09 g (20.2 mmol) of L-valinol in 10 mL of methylene chloride was added to a solution of 3.71 g (16.9 mmol) of 2-(2-furanyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one in 100 ml of toluene, and the mixture was heated under reflux for 14 hours. The reaction solution was concentrated under reduced pressure, ethyl acetate was added to the residue, and the mixture was washed with water, a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and then saturated brine. The organic layer was dried with anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. Ethyl acetate was added to the residue, and the mixture was stirred overnight. The obtained crystal was collected by filtration to obtain 4.06 g (74.7%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08829209B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-6405efd6ebeb41a4b29260cd120c5ea8 |
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| 출처 메모 | uspto-grants-2014_09 |
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