関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | 3,5-Dibromo-2-methylpyridine | HCID 619705 | — |
| 反応物 | 1-methyl-5-(tributylstannyl)-1H-pyrazolo[4,3-b]pyridine | HCID 86700155 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-(5-bromo-2-methylpyridin-3-yl)-1-methyl-1H-pyrazolo[4,3-b]pyridine | HCID 86700455 | — |
反応手順
To a solution of 3,5-dibromo-2-methylpyridine (320 mg, 1.28 mmol) in dioxane (10 mL), was added 1-methyl-5-(tributylstannyl)-1H-pyrazolo[4,3-b]pyridine (540 mg, 1.28 mmol), CuI (73 mg, 0.38 mmol), LiCl (271 mg, 6.4 mmol) and Pd(PPh3)4 (147 mg, 0.12 mmol). The reaction mixture was heated at 100° C. for 2 h. The reaction was cooled down, washed by sat. NaHCO3, extracted by EtOAc, dried over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-100% EtOAc in hexanes give the product. LCMS-ESI+: calc'd for C13H11BrN4: 303.0 (M+H+); Found: 303.2 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987250B2 |
|---|
| 出典データセット | uspto-grants-2015_03 |
|---|
| ORD ID | ord-8e01976eaffd47d09812a762b433d697 |
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| 出典メモ | uspto-grants-2015_03 |
|---|
