関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidin-4-ol | HCID 79341 | — |
| 反応物 | 6-Chloro-2-methyl-2,3-dihydropyridazin-3-one | HCID 2783607 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diisopropylethylamine | HCID 81531 | — |
| 生成物 | 6-(4-hydroxypiperidin-1-yl)-2-methylpyridazin-3(2H)-one | HCID 86721994 | 83% |
反応手順
To a slurry of 6-chloro-2-methylpyridazin-3(2H)-one (1 g, 6.94 mmol) in DIPEA (20 mL) was added piperidin-4-ol (0.84 g, 8.33 mmol) and the reaction mixture was stirred at 120° C. overnight. The resulting mixture was diluted with water (30 mL) and extracted with DCM (3×30 mL) to remove impurities. The aqueous phase was concentrated to dryness to afford the title compound as a yellow solid (1.2 g, 83%). [LCMS: Rt=1.07 min, m/z 210.1 (M+H)]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09034874B2 |
|---|
| 出典データセット | uspto-grants-2015_05 |
|---|
| ORD ID | ord-447dff96b2014eeb82a2992dbfbd8559 |
|---|
| 出典メモ | uspto-grants-2015_05 |
|---|
