化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → [2-Ethyl-5-(trifluoromethyl)phenyl]boronic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Trimethyl borate | HCID 8470 | — |
| 反応物 | 1-Ethyl-2-iodo-4-(trifluoromethyl)benzene | HCID 70980748 | — |
| 反応物 | HCID 178418918 | HCID 178418918 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [2-Ethyl-5-(trifluoromethyl)phenyl]boronic acid | HCID 66571440 | — |
反応手順
i-Propylmagnesium chloride (2M sol. in THF, 5.81 mL, 11.6 mmol) was added drop wise to a cooled (−30° C.) solution of 2-iodo-1-ethyl-4-(trifluoromethyl)benzene (3.48 g, 11.6 mmol) in dry THF (30 mL) and the reaction mixture was stirred at the same temperature for 30 min, under argon. After this time, trimethylborate (2.6 mL, 23.2 mmol) was added drop wise and the reaction mixture was stirred at the same temperature for 1.5 h. HCl (1 M, 10 mL) was added and the reaction mixture extracted with EtOAc (3×40 mL). The combined organic layers were dried over sodium sulfate and the solvent was evaporated to obtain the title compound as a white solid, crystallized from hexane (2.46 g, 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09283224B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-324728e2e5fa46618cad2b61b0de3f9a |
| 出典メモ | uspto-grants-2016_03 |