참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | 2-Bromo-6-methylpyridine 1-oxide | HCID 3652084 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 2-Bromo-6-methyl-4-nitro-1-oxo-1lambda~5~-pyridine | HCID 2751816 | 57% |
반응 단계
To cooled nitric acid (concentrated, 168 ml) was added sulfuric acid (concentrated, 300 ml) under cooling followed by 2-bromo-6-methyl-pyridine 1-oxide (35 g, 0.186 mol). The mixture was stirred at 70° C. for 4 hours, cooled to room temperature and poored slowly on crushed ice. A stream of nitrogen was bubbled through the mixture overnight. The mixture was basified to pH 8 under cooling with NaOH (10N, ca. 1 L), diluted with water (3 L) and extracted with DCM (5×). The combined organic phases were dried (sodium sulfate) and evaporated to dryness to yield 27.6 g of a yellow crystaline solid (0.118 mol, 57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09321724B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-970edf86b814412faf18b6f7474e2814 |
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| 출처 메모 | uspto-grants-2016_04 |
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