関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Bromo-2-nitrophenol | HCID 24364 | — |
| 反応物 | 3-Pyridinylboronic acid | HCID 2734378 | — |
| 触媒 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Sodium Carbonate | HCID 10340 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-(4-Methyl-2-nitro-phenyl)-pyridine | HCID 11745972 | — |
反応手順
4-Bromo-2-nitro-phenol (648 mg, 3.0 mmol) and 3-pyridyl boronic acid (387 mg, 3.15 mmol) were diluted with 5 mL of dioxane and placed under N2. Potassium carbonate was diluted in 1 mL of H2O and added to the reaction mixture. Tetrakis(triphenylphosphine) palladium (173 mg, 0.15 mmol) was added, then the reaction was heated to 70° C. and stirred overnight. The reaction was allowed to cool to room temperature, then diluted with 30 mL of EtOAc and 30 mL of 10% Na2CO3. The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The material was purified with a Biotage 40M cartridge eluting with hexanes/EtOAc, 1/1 to yield an off white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560462B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-1cd7e63882694d8b92fa652bbf8ab09d |
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| 出典メモ | uspto-grants-2009_07 |
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