참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-Methylpiperazine | HCID 53167 | — |
| 반응물 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Methyl-4-(5-nitropyridin-2-yl)piperazine | HCID 2764066 | 90% |
반응 단계
A stirred mixture of 2-chloro-5-nitropyridine (3.16 g, 20.0 mmol), 1-methyl-piperazine (2.00 g, 2.00 mmol) and potassium carbonate (2.76 g, 20.0 mmol) in DMF is heated at 100° C. for 24 h, cooled, poured into water and extracted with CH2Cl2. The combined extracts are dried over MgSO4 and concentrated in vacuo. The resultant residue is purified by flash chromatography (SiO2, 2% ammonia in 10:90 ethanol:ethyl acetate as eluent) affords the title compound as an off-white solid, 4.0 g (90% yield), identified by NMR analysis.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07259165B2 |
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| 출처 데이터셋 | uspto-grants-2007_08 |
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| ORD ID | ord-ffc0e54e765c4103a76baaa42ef2a001 |
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| 출처 메모 | uspto-grants-2007_08 |
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