関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylsilane | HCID 12052 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Bromo-4'-methoxybenzophenone | HCID 794333 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 4-Methoxy(4-bromo-benzyl)-benzene | HCID 13704006 | 101.5% |
反応手順
To a solution of the product from step 1 (0.5 g, 1.6 mmol) in TFA (1 mL) was added triethylsilane (0.5 mL, 25 mmol) at 0° C. The resulting mixture was allowed to warm to rt and stir at rt for 16 h. The mixture was poured onto 30 mL ice-water solution, neutralized with aq NaOH (2N) to pH=6-7, and then extracted with EtOAc (2×20 mL). The combined organic layers were washed with water (5×20 mL) and brine (20 mL). and dried over anhy. Na2SO4. The solvent was removed in vacuo to obtain the crude product which was purified by silica gel flash chromatography to afford the title product (0.45 g, 85%) as a solid; 1H NMR (400 MHz, CDCl3); δ 3.78 (s, 3H), 3.87 (s, 2H), 6.82 (d, J=8.8, 2H), 7.04 (d, J=8.8, 2H), 7.07 (d, J=8.8, 2H), 7.98 (d, J=8.4, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07402684B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-8b56f401018e47cba67a82a3d599670c |
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| 出典メモ | uspto-grants-2008_07 |
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