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Toluene → 2-Bromo-1-[3-(trifluoromethyl)phenyl]ethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 3'-(Trifluoromethyl)acetophenone | HCID 67682 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-1-[3-(trifluoromethyl)phenyl]ethan-1-one | HCID 2778386 | 81.8% |
反応手順
To a toluene solution (423 mL) of commercially available 3′-trifluoromethylacetophenone (79.6 g, 0.423 mol) was added pyridinium bromide perbromide (135.4 g, 0.423 mol) under ice cooling and stirred for 5 hours while heating up to room temperature. The reaction liquid was ice cooled again, followed by dropwise adding 400 mL of distilled water to stop reaction and fractionation. A toluene layer was washed with 400 mL of a saturated aqueous solution of sodium bicarbonate, followed by drying with magnesium sulfate anhydride and concentration under reduced pressure and distillation under reduced pressure to obtain an objective compound (92.35 g, 81.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07563893B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-1563afc41a58401c95a39af9048a3f05 |
| 出典メモ | uspto-grants-2009_07 |