関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium fluoride | HCID 25953 | — |
| 反応物 | 2-(Tributylstannyl)pyridine | HCID 607784 | — |
| 反応物 | 3-Bromo-6-methylpyridine-2-carbonitrile | HCID 21952747 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6'-Methyl-2,3'-bipyridine-2'-carbonitrile | HCID 59363716 | 88% |
反応手順
A mixture of 3-bromo-6-methylpicolinonitrile (1 g, 5.1 mmol), 2-(tributylstannyl)pyridine (2.43 ml, 6.60 mmol), cesium fluoride (150 mg, 10.2 mmol), CuI (193 mg, 1.02 mmol) and Pd(PPh3)4 (586 mg, 0.51 mmol) in DMF (10 mL) was degassed and heated at 120° C. for 1 h in a microwave reactor. The solvent was removed in vacuo to obtain the crude which was purified by silica gel chromatography (0˜100% DCM/EtOAc) to yield the title compound as a brown oil (0.87 g, 88%). MS (ESI) 196 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440982B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-ca8ed7fd06cf4ff3a8a7b5ac5854dc1b |
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| 出典メモ | uspto-grants-2016_09 |
|---|
