関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2,3,4-Trifluorophenol | HCID 123174 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-(Benzyloxy)-2,3,4-trifluorobenzene | HCID 83396906 | 90.7% |
反応手順
Sodium carbonate (19.50 g, 183.96 mmol) was dispersed into a solution of 2,3,4-trifluorophenol (13.64 g, 92.10 mmol) in acetone (300 mL). To the stirred suspension was added benzyl bromide (17.31 g, 101.21 mmol) dropwisely. The mixture was heated under reflux at 50° C. for 24 h. The acetone was removed under reduced pressure and the residue was dissolved in water (300 mL). The solution was extracted with ethyl acetate (100 mL×2). The combined organic extracts were washed with 5% sodium hydroxide (100 mL) and brine (100 mL) sequentially and dried over Na2SO4. The solvent was removed in vacuo to yield a pale yellow solid (19.89 g, 90.7% yield). 1H NMR (400 MHz, CDCl3): δ 7.40 (m, 5H), 6.85 (m, 1H), 6.64 (m, 1H), 5.15 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09290468B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-02b6d58abe6a43db8f199e07bb9a2740 |
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| 出典メモ | uspto-grants-2016_03 |
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