참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 반응물 | 1-(4-Methoxyphenyl)-piperazine, dihydrochloride | HCID 2723700 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 1-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine | HCID 3742676 | 57.4% |
반응 단계
A mixture of 36 g of 1-(4-methoxyphenyl)piperazine dihydrochloride, 22 g of 2-chloro-5-nitropyridine, 58 g of potassium carbonate and 227 ml of dimethyl sulfoxide was stirred overnight at 140° C. The reaction mixture was cooled and poured onto water. The precipitated product was filtered off, washed with water and dissolved in dichloromethane. The solution was treated with activated charcoal. The latter is filtered off and the filtrate was evaporated. The residue was triturated in 2-propanol. The product was filtered off and crystallized from 1-butanol, yielding 24.5 g of 1-(4-methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine; mp. 170° C. (interm. 21).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05650411 |
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| 출처 데이터셋 | uspto-grants-1997_07 |
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| ORD ID | ord-0a116ba728584cf7b32d9a1d3add1357 |
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| 출처 메모 | uspto-grants-1997_07 |
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