참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 반응물 | 5-Bromo-2-nitropyridine | HCID 817620 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Tert-butyl 4-(6-nitropyridin-3-yl)piperazine-1-carboxylate | HCID 11243758 | 33% |
반응 단계
A solution is prepared of 1 g (4.9 mM) of 2-nitro-5-bromopyridine and 917 mg (4.9 mM) of N-Boc-piperazine in 10 ml of dimethylformamide and 1.02 g (7.4 mM) of potassium carbonate are added. The reaction mixture is agitated at 120° C. for 36 hours and then cooled. 50 ml of water are then added and extraction is carried out with ethyl acetate. The organic phase obtained is washed with water, dried and concentrated under reduced pressure. The crude product is purified by silica gel chromatography in eluting with the aid of a toluene/isopropanol mixture (98/2; v/v). The product sought after is thus obtained as a yellow solid (yield=33%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07538111B2 |
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| 출처 데이터셋 | uspto-grants-2009_05 |
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| ORD ID | ord-be504eb9429b40eaa9d3ea8ff4b4dd3b |
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| 출처 메모 | uspto-grants-2009_05 |
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