関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromophenol | HCID 11563 | — |
| 反応物 | 4-(Bromomethyl)phenylboronic acid | HCID 2735593 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | [4-[(3-Bromophenoxy)methyl]phenyl]boronic acid | HCID 67975234 | 50.8% |
反応手順
3-bromophenol (0.50 g) was dissolved in acetone, and to the resultant solution, potassium carbonate (1.49 g), potassium iodide (14 mg), and 4-bromomethylphenyl boronic acid (0.62 g) were added, followed by heating the resultant reaction mixture under reflux for 3 hours. The reaction mixture was left to be cooled down, and to the reaction mixture, water was added, and a 2M hydrochloric acid was added to adjust pH of the reaction mixture to 2 to 3, followed by extracting the reaction mixture with ethyl acetate. The organic phase was washed with saturated saline and was dried over anhydrous sodium sulfate. From the organic phase, the solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography to obtain the subject compound (0.45 g) as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476287B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-863fe1b89fa74fa7a3f641d3e8940456 |
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| 出典メモ | uspto-grants-2013_07 |
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