참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 2-Bromo-6-methylpyridine 1-oxide | HCID 3652084 | — |
| 생성물 | 2-Bromo-6-methyl-4-nitro-1-oxo-1lambda~5~-pyridine | HCID 2751816 | 40% |
반응 단계
Concentrated nitric acid (4 mL) was added to cold concentrated sulfuric acid (7 mL). 2-Bromo-6-methyl-pyridine 1-oxide (820 mg, 4.36 mmol) was added to this and then heated at 70° C. for 4 h. The mixture was cooled and poured slowly into ice-cold water (100 mL) and basified to pH ˜8 with sodium bicarbonate solution. This was extracted with ethyl acetate (4×50 mL) then the combined organic layers were dried over anhydrous sodium sulfate and concentrated to give a residue which was purified by washing with pentane (50 mL) to afford 2-bromo-6-methyl-4-nitro-pyridine 1-oxide (0.41 g, 40%) as a free flowing yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08524705B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-9f7ac09e91f147b1838c657ff9dbbc63 |
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| 출처 메모 | uspto-grants-2013_09 |
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