関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,5-Dibromopyridine | HCID 69353 | — |
| 反応物 | 3-Fluoro-4-(tributylstannyl)pyridine | HCID 22273601 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Bromo-3'-fluoro-2,4'-bipyridine | HCID 58415812 | 62% |
反応手順
In a schlenck tube, a mixture of 2,5-dibromopyridine (2.11 mmol, 0.500 g), 3-fluoro-4-(tributylstannyl)pyridine (2.32 mmol, 0.896 g), PdCl2(PPh3)2 (0.21 mmol, 0.148 g), CuI (0.43 mmol, 0.080 g) in DMF (5 ml) was heated at 130° C. for 12 hours, under argon atmosphere. The solvent was evaporated and the crude mixture was extracted between water and ethyl acetate. The solid residue was purified by chromatography over SiO2 eluting with DCM/methanol mixtures affording 0.330 g (yield 62%) of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08536165B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-a11cea2e8f2340d298289a02033d0720 |
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| 出典メモ | uspto-grants-2013_09 |
|---|
