참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-Amino-2,6-dichloropyridine | HCID 137652 | — |
| 생성물 | 2,6-Dichloro-4-nitraminopyridine | HCID 421617 | — |
반응 단계
2,6-dichloropyridin-4-amine (100 g, 0.617 mol) was added slowly to conc. H2SO4 (415 mL) by portion while cooled with an ice bath. The mixture was cooled to 0° C., and nitric acid (250 mL) was added dropwise at 0° C. The mixture was stirred at room temperature for 2 h. TLC (petroleum ether/ethyl acetate=2:1) showed the reaction was complete. The mixture was poured into crushed ice and stirred for 30 min. The resulting precipitate was collected by filtration and washed with water to give crude N-(2,6-dichloropyridin-4-yl)nitramide as a yellow solid, which was used for the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846657B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-05adcfb6810f41fbbbef635f537c4b81 |
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| 출처 메모 | uspto-grants-2014_09 |
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