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 | 90.8% |
反応手順
Sodium carbonate (19.50 g, 0.184 mol) was dispersed into a solution of 2,3,4-trifluorophenol (13.64 g, 0.092 mol) in acetone (300 mL). To the stirred suspension was added the solution of benzyl bromide (17.31 g, 101.21 mmol) in acetone (100 mL) dropwisely. The mixture was heated under reflux at 50° C. for 24 h, allowed to cool to room temperature, and filtered. The filter cake was washed with acetone (50 mL×3), and acetone was removed under reduced pressure. The residue was dissolved in ethyl acetate (500 mL). The solution was washed with 5% sodium hydroxide (50 mL), water (150 mL) and brine (150 mL) sequentially and dried over Na2SO4. The solvent was removed in vacuo to yield a pale yellow solid (19.89 g, 90% 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-6131eb85bf16441fadf990c4325637fa |
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| 出典メモ | uspto-grants-2016_03 |
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