関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 2,6-Dichloroisonicotinonitrile | HCID 735906 | — |
| 反応物 | 2-[(4-fluorophenyl)sulfonyl-ethyl-amino]-N-[[2-[4-(trifluoromethoxy)phenyl]-4-pyridyl]methyl]prop-2-enamide | HCID 78319909 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | 2-[(5-chloro-2-thienyl)sulfonyl-ethyl-amino]N-[[2-[4-(trifluoromethoxy)phenyl]-4-pyridyl]methyl]prop-2-enamide | HCID 78319913 | — |
| 生成物 | 2-Chloro-6-morpholin-4-yl-isonicotinonitrile | HCID 83074581 | 89% |
反応手順
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)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09409864B2 |
|---|
| 出典データセット | uspto-grants-2016_08 |
|---|
| ORD ID | ord-aa930a730be148839c0def30ec789bd8 |
|---|
| 出典メモ | uspto-grants-2016_08 |
|---|
