참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Imidazole | HCID 795 | — |
| 반응물 | 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine | HCID 19935587 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 3-Amino-4,5-diethoxycarbonyl-6-(imidazol-1-yl)-2-phenylpyridine | HCID 15289700 | 89.8% |
반응 단계
A mixture of 0.379 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.21 g of imidazole and 15 ml of chloroform was heated under reflux for 8 hours. After the reaction mixture was concentrated, the residue was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. After the solvent was distilled off, 5 ml of acetic acid and 0.5 g of reduced iron were added to the residue, and the mixture was stirred at room temperature for 4 hours. After an aqueous solution of sodium hydrogencarbonate was added for neutralization, extraction with ethyl acetate was conducted. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate, followed by filtration with a small amount of silica gel. The filtrate was concentrated under reduced pressure, to give 0.342 g of the title compound as a yellow oily substance.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05420275 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-78b21301283c45709220707c2c207948 |
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| 출처 메모 | uspto-grants-1995_05 |
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