참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-Bromo-6-chloro-2-fluorophenol | HCID 66601002 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1-Bromo-4-chloro-2-fluoro-3-methoxybenzene | HCID 66600367 | — |
반응 단계
To a stirred solution of 3-bromo-6-chloro-2-fluorophenol (4.2 g, 18.63 mmol) in acetonitrile (35 mL) was added potassium carbonate (5.15 g, 37.3 mmol) followed by the addition of methyl iodide (2.330 mL, 37.3 mmol) dropwise at rt. The reaction mixture was heated to 85° C. for 3 h. The volatiles were evaporated; water (50 mL) was added and the solution extracted with ethyl acetate (2×80 mL). The combined organic layers were washed with brine (100 mL), dried over sodium sulphate, and concentrated under reduced pressure. The crude material was taken to the next step without further purification. 1H NMR (400 MHz, CDCl3) δ 7.20 (m, 1H), 7.05 (m, 1H), 3.98 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08969564B2 |
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| 출처 데이터셋 | uspto-grants-2015_03 |
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| ORD ID | ord-d19569144d3d4a89b2e8a0fdb291a997 |
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| 출처 메모 | uspto-grants-2015_03 |
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