참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | 2,6-Dichloroisonicotinonitrile | HCID 735906 | — |
| 반응물 | 2-[(4-fluorophenyl)sulfonyl-ethyl-amino]-N-[[2-[4-(trifluoromethoxy)phenyl]-4-pyridyl]methyl]prop-2-enamide | HCID 78319909 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | 2-[(5-chloro-2-thienyl)sulfonyl-ethyl-amino]N-[[2-[4-(trifluoromethoxy)phenyl]-4-pyridyl]methyl]prop-2-enamide | HCID 78319913 | — |
| 생성물 | HCID 83074581 | HCID 83074581 | 89% |
반응 단계
2,6-dichloropyridine-4-carbonitrile 24 (4 gr, 23.13 mmol) was dissolved in 100 ml of ethanol. To the solution were added TEA (1 equiv., 3.22 ml), morpholine (1 equiv., 2 ml) and the mixture was stirred at 70° C. for 4 hours. (TLC AcOEt 3/petroleum ether 7). The solvent was evaporated and the residue was dissolved with ethyl acetate, washed with water and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The crude was crystallized from ethyl acetate and petroleum ether to give a beige solid. (4.6 g, 89% yield) 1HNMR (DMSO, 400 MHz) δ 3.58 (4H, m), 3.64 (4H, m), 7.10 (1H, s), 7.32 (1H, s)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09409864B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_08 |
|---|
| ORD ID | ord-aa930a730be148839c0def30ec789bd8 |
|---|
| 출처 메모 | uspto-grants-2016_08 |
|---|
