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 | Benzene, 2-chloro-1-fluoro-4-(trifluoromethyl)- | HCID 157153 | — |
| 反応物 | 4-Hydroxyphenylboronic acid | HCID 2734360 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | [4-[2-Chloro-4-(trifluoromethyl)phenoxy]phenyl]boronic acid | HCID 67972395 | 13.2% |
反応手順
A solution of 2-chloro-1-fluoro-4-(trifluoromethyl)benzene (0.95 g), (4-hydroxyphenyl)boronic acid (0.66 g), and potassium carbonate (1.65 g) in DMSO (5.0 mL) was heated with stirring at 130° C. for 20 hours. The resultant reaction mixture was left to be cooled down and was poured into an ice water, and pH of the resultant reaction mixture was adjusted to around 2 with a 10% hydrochloric acid, followed by extracting the reaction mixture with ethyl acetate. From the organic phase, the solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography (eluate; n-hexane:ethyl acetate 100:0 to 50:50) to obtain the subject compound (0.20 g) as a white 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-41a8d61ec7344509a0cbc969aa69eb85 |
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| 出典メモ | uspto-grants-2013_07 |
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