関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Fluoro-4-nitrophenol | HCID 9825 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-(7-Chlorothieno[3,2-b]pyridin-2-yl)-1-(2-morpholinoethyl)pyrimidin-2(1H)-one | HCID 58790088 | — |
| 溶媒 | Diphenyl Ether | HCID 7583 | — |
| 生成物 | HCID 58790417 | HCID 58790417 | 26% |
反応手順
To a solution of the pyridone 414 (236 mg, 0.63 mmol) in Ph2O (1.3 mL) was added 2-fluoro-4-nitrophenol (197 mg, 1.26 mmol) and K2CO3 (173 mg, 1.26 mmol). The mixture was stirred at 100° C. for 1 h, then at 180° C. for 2 h, cooled and evaporated under reduced pressure. The residue was purified by flash chromatography with a gradient of methanol (2-10%) in dichloromethane to give title compound 415 (81 mg, 26% yield). MS (m/z): 498.0 (M+H). 1H NMR (DMSO-d6) δ (ppm): 9.16 (d, J=3.3 Hz, 1H), 8.66 (d, J=3.3 Hz, 1H), 8.60 (d, J=5.3 Hz, 1H), 8.47 (dd, J=10, 2.5 Hz, 1H), 8.19 (d, J=8.8 Hz, 1H), 8.02 (s, 1H), 7.69 (t, J=8.6 Hz, 1H), 6.98 (d, J=5.3 Hz, 1H), 4.02 (t, J=5.5 Hz, 2H), 3.58-3.43 (m, 4H), 2.59 (t, J=5.5 Hz, 2H), 2.50-2.41 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08329726B2 |
|---|
| 出典データセット | uspto-grants-2012_12 |
|---|
| ORD ID | ord-6fdb92ed9c3f4eaea48576127274a816 |
|---|
| 出典メモ | uspto-grants-2012_12 |
|---|
