참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| 반응물 | Dimethylamine tetrahydrofuran | HCID 22320367 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-Chloro-2-dimethylamino-3-nitropyridine | HCID 21787625 | 52.1% |
반응 단계
A mixture of 2,6-dichloro-3-nitropyridine (1.9 g, 10 mmole) and potassium carbonate (1.66 g, 12 mmole) in 30 ml of tetrahydrofuran was stirred at 0° C. for 5 min. A solution of dimethylamine/tetrahydrofuran (2M, 6 ml, 12 mmole) was added dropwise to the reaction mixture over 40 min. After stirring for 5 min at 0° C., the mixture was warmed to room temperature and stirred overnight. The reaction mixture was filtered and the filtrate was collected and concentrated under reduced pressure. The crude product was purified by flash chromatography, eluting with 87% hexane: 13% ethyl acetate to give 6-chloro-2-dimethylamino-3-nitro pyridine (1.05 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07425557B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-db7404d2ea0440ff97a6c636cfbf6052 |
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| 출처 메모 | uspto-grants-2008_09 |
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