関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(Trifluoromethyl)phenylboronic acid | HCID 2734389 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 反応物 | 2-Iodo-3-methoxy-6-methylpyridine | HCID 11482051 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Methoxy-6-methyl-2-(4-(trifluoromethyl)phenyl)pyridine | HCID 58443268 | — |
反応手順
To a mixture of 4-(trifluoromethyl)phenylboronic acid (0.97 g, 5.1 mmol), S—PHOS (0.20 g, 0.47 mmol), potassium carbonate (2.0 g, 15 mmol), and Pd(OAc)2 (0.061 g, 0.27 mmol) was added a solution of 2-iodo-3-methoxy-6-methylpyridine (prepared in the previous step) in acetonitrile (6 mL) followed by water (4 mL). The reaction mixture was degassed by bubbling nitrogen through the solution for 10 min, and the reaction mixture was heated to 75° C. After 4 h, the reaction mixture was diluted with EtOAc, washed with saturated NaHCO3 (1×), brine (1×), dried over MgSO4, filtered, and concentrated. Purification by flash column chromatography on silica gel (5% to 20% EtOAc in hexanes) gave 3-methoxy-6-methyl-2-(4-(trifluoromethyl)phenyl)pyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08791147B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-0efef0adc9b44a178b643bef49bc58a1 |
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| 出典メモ | uspto-grants-2014_07 |
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