참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Pyridine, 2-methyl-4-nitro-, 1-oxide | HCID 95291 | — |
| 반응물 | 4-Bromo-3-fluorophenol | HCID 2779153 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-(4-Bromo-3-fluorophenoxy)-2-methylpyridine 1-oxide | HCID 59287312 | — |
반응 단계
4-Bromo-3-fluorophenol (0.5 g, 2.61 mmol) was added to a solution of sodium hydride (0.115 g, 2.90 mmol) in DMF (5 ml). After stiffing for 10 minutes 4-nitro-2-picoline N-oxide (0.37 g, 2.41 mmol) was added. The reaction mixture was heated at 180° C. for 1 hour under microwave irradiation. After cooling to room temperature the mixture was filtered through diatomaceous earth and this was thoroughly washed with EtOAc. The filtrate was washed with water (2×25 ml), the organic fraction was dried (Na2SO4) and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; 0-3% methanol/DCM as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate D12 (0.33 g, 49%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08748621B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-1dcfdd3f566349dbb75c98d9510b130b |
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| 출처 메모 | uspto-grants-2014_06 |
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