関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Dichlorophenol | HCID 7258 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,5-Difluorobenzonitrile | HCID 123558 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(3,4-Dichlorophenoxy)-5-Fluoro-Benzonitrile | HCID 22019275 | — |
反応手順
A flame-dried flask containing N2 inlet and magnetic stirrer was charged with 2.9 g (18 mmol) of 3,4-dichlorophenol, 6.2 g (45 mmol) of potassium carbonate and 50 mL of anhydrous DMF. With stirring, 2.08 g (15 mmol) of 2,5-difluorobenzonitrile (Aldrich Chem. Co.) was added and the mixture was heated overnight at 105° C., cooled to room temperature and partitioned between water and EtOAc. The aqueous layer was reextracted with EtOAc and the combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl. After drying with MgSO4, the solvent was removed to give the title product as a light brown oil which slowly solidified, 3.5 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084165B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-46b34f726ee24169b4da1dd46149cf32 |
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| 出典メモ | uspto-grants-2006_08 |
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