化工社化工社 化学情報印刷レポート · 研究参考用
3',5'-Difluoroacetophenone → 2-(3,5-Difluorophenyl)propan-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3',5'-Difluoroacetophenone | HCID 518596 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(3,5-Difluorophenyl)propan-2-ol | HCID 57732159 | — |
反応手順
A solution of 1-(3,5-difluoro-phenyl)-ethanone (156 g, 1 mol, 1 eq) in THF (500 mL) was added dropwise under argon to the commercially available solution of methymagnesium bromide (143 g, 1.2 mol, 1.2 eq) in THF at such a rate that gentle refluxing was maintained. After the addition was complete the reaction mixture was stirred at ambient temperature for an hour and poured into ice-cold aqueous saturated ammonium chloride. Phases were separated and aqueous layer extracted two times with ethyl acetate. The combined organic layers were washed with brine and dried over anhydrous magnesium sulfate. After removal of the solvent title compound was purified by distillation under reduced pressure (145 g, 0.84 mol, 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741934B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-a1eb185159174766a70ab795d9073411 |
| 出典メモ | uspto-grants-2014_06 |