関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | (3-Methoxyphenyl)boronic acid | HCID 2734370 | — |
| 反応物 | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Fluoro-3'-methoxy-3-nitrobiphenyl | HCID 10490702 | — |
反応手順
4-Bromo-1-fluoro-2-nitro-benzene (5 gms.), 3.85 gms. 3-methoxyphenylboronic acid and 22 mL of a 2M aqueous solution of sodium carbonate are suspended in 100 mL of a 1:1 (v:v) mix of toluene and ethanol. The resulting suspension is then treated with 0.8 gms. tetrakis(triphenylphosphine)palladium(0) at room temperature. The reaction mixture is then heated at reflux for 12 h. The reaction mixture is subsequently concentrated in vacuo, and the resulting residue is taken up in ethyl acetate (200 mL). The ethyl acetate solution is then washed successively with water (2×200 mL), and brine (2×200mL). The organic layer is then dried by filtering through phase separator paper and concentrated in vacuo to yield 7.19 gms. of crude product. The crude product is then recrystallized from hot ethanol yielding 4-fluoro-3′-methoxy-3-nitro-biphenyl as a yellow-white solid in the amount of 4.767 gms.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098236B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-842c8a1fc9d040ed9e1571297c6d1a76 |
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| 出典メモ | uspto-grants-2006_08 |
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