참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 반응물 | 4-Amino-3-Nitrophenol | HCID 3758882 | — |
| 반응물 | 4-chloro-N,N-dimethylpyridine-2-carboxamide | HCID 4962252 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-(4-Amino-3-nitro-phenoxy)-pyridine-2-carboxylic acid dimethylamide | HCID 21037294 | — |
반응 단계
A mixture containing 4-amino-3-nitrophenol (1 eq) and potassium bis(trimethylsilyl)amide (2 eq) was stirred in dimethylformamide for 2 hours at room temperature. To this mixture was added 4-Chloro-pyridine-2-carboxylic acid dimethylamide (1 eq) and potassium carbonate (1.2 eq) and then it was stirred at 90° C. for 3 days. The reaction mixture was then concentrated before partitioning between ethyl acetate and water. The organic layer was separated, washed with brine, dried, filtered and concentrated in vacuum to give brown solid. Purification by flash chromatography with ethyl acetate and hexane (1:1) gave the desired product as a yellow syrup. HPLC, 1.69 min; MS: MH+=303.1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07728010B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-2ce32362d15346048dc575b0b0923ee7 |
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| 출처 메모 | uspto-grants-2010_06 |
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