참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | (3-Methoxyphenyl)boronic acid | HCID 2734370 | — |
| 반응물 | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4-Fluoro-3'-methoxy-3-nitrobiphenyl | HCID 10490702 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07098236B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-842c8a1fc9d040ed9e1571297c6d1a76 |
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| 출처 메모 | uspto-grants-2006_08 |
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