関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrazole | HCID 1048 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 5-Amino-2-fluoropyridine | HCID 819440 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 6-(1H-pyrazol-1-yl)pyridin-3-amine | HCID 16774822 | 17% |
反応手順
Commercial 6-fluoropyridin-3-amine (500 mg, 4.46 mmol) was dissolved in 20 mL dry NMP. To it were added pyrazole (910 mg, 13.4 mmol) and cesium carbonate (4.4 g, 13.4 mmol). The mixture was stirred in a sealed tube at 120° C. for over the weekend (3 nights). The mixture was diluted with chloroform, washed with brine (3 times), dried, concentrated and subjected to flash column (0 to 30% EtOAc in DCM) to isolate 6-(1H-pyrazol-1-yl)pyridin-3-amine (120 mg, 17% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846928B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-b211c993c0db4887b1819cb46fe63efb |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
