関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,5-Dibromo-2-methylpyridine | HCID 619705 | — |
| 反応物 | 5-(Bromomethyl)-1-methyl-1H-indazole | HCID 49761704 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-(5-bromo-2-methylpyridin-3-yl)-1-methyl-1H-indazole | HCID 86700366 | — |
| 生成物 | 5-(5-bromo-6-methylpyridin-3-yl)-1-methyl-1H-indazole | HCID 86700367 | — |
反応手順
To a solution of 3,5-dibromo-2-methylpyridine (1.0 g, 3.99 mmol) and 5-(bromomethyl)-1-methyl-1H-indazole (772 mg, 4.38 mmol) in 1,4-dioxane (12 mL) was added Pd(PPh3)4 (231 mg, 0.20 mmol) and potassium carbonate solution (2 M aqueous, 6 mL, 12 mmol). The reaction mixture was stirred at 105° C. in a sealed tube for 1.5 h. The mixture was diluted with water (15 mL) and EtOAc (20 mL). The layers were separated, and the organic layer was dried, filtered, and concentrated in vacuo. The crude material was purified by CombiFlash (EtOAc w/5% MeOH and Hexanes) to give 5-(5-bromo-2-methylpyridin-3-yl)-1-methyl-1H-indazole and 5-(5-bromo-6-methylpyridin-3-yl)-1-methyl-1H-indazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987250B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-ca3fabd5a2aa4e58945490cc7b3a090f |
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| 出典メモ | uspto-grants-2015_03 |
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