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Cesium carbonate → 3-(6-Chloro-3-methylpyridazin-4-yloxy)pyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Amino-3-Hydroxypyridine | HCID 28114 | — |
| 反応物 | 4,6-Dichloro-3-methylpyridazine | HCID 58717049 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(6-Chloro-3-methylpyridazin-4-yloxy)pyridin-2-amine | HCID 86641108 | 55.7% |
反応手順
2-Aminopyridin-3-ol (5.0 g, 45.4 mmol) and 4,6-dichloro-3-methylpyridazine (7.4 g, 45.4 mmol, prepared according to WO 2003/041712) were dissolved in DMSO (100 mL). Cs2CO3 (16.3 g, 49.9 mmol) was added and the reaction stirred at ambient temperature for one hour. The reaction was diluted with water and the material was extracted with CH2Cl2, dried (Na2SO4), filtered and concentrated. Flash chromatography followed by trituration of the concentrated solid with EtOH gave 3-(6-chloro-3-methylpyridazin-4-yloxy)pyridin-2-amine (5.98 g, 25.3 mmol, 55%) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08362037B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-26fdc25a0e444202a9bdfbe14c9feaac |
| 出典メモ | uspto-grants-2013_01 |