참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 반응물 | N-(3-hydroxyphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide | HCID 19481482 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1,3-dimethyl-N-{3-[(5-nitropyridin-2-yl)oxy]phenyl}-1H-pyrazole-5-carboxamide | HCID 57749382 | 98.3% |
반응 단계
A mixture of N-(3-hydroxyphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide (1.58 g, 6.83 mmol), 2-chloro-5-nitropyridine (1.03 g, 6.51 mmol), potassium carbonate (1.42 g, 10.2 mmol) and N,N-dimethylformamide (10 mL) was stirred at 60° C. for 15 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was purified by column chromatography (hexane/ethyl acetate=70/30→0/100) to give the title compound (2.26 g, 94%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08304557B2 |
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| 출처 데이터셋 | uspto-grants-2012_11 |
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| ORD ID | ord-418d69c0ffec416197ccf63349b6402e |
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| 출처 메모 | uspto-grants-2012_11 |
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