참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,3-Dichloropyridine | HCID 16988 | — |
| 반응물 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 촉매 | Copper | HCID 23978 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Tert-butyl 4-(3-chloropyridin-2-yl)piperazine-1-carboxylate | HCID 11630777 | — |
반응 단계
A mixture of 2,3-dichloropyridine (10 g, 67.5 mmol, Aldrich), tert-butyl 1-piperazinecarboxylate (12.58 g, 67.5 mmol, Aldrich), copper powder (0.5 g, 7.8 mmol) and K2CO3 (9.33 g, 67.5 mmol) in DMF (100 mL) was stirred at 120° C. for 16 h. The reaction mixture was cooled to room temperature, concentrated in vacuo and the residue was dissolved in EtOAc (200 mL). The organic solution was washed with saturated aqueous solution of NaHCO3 (50 mL) and brine (50 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel column chromatography, eluting with 15% EtOAc/hexane, to give the title compound as an orange oil. MS (ESI, pos. ion) m/z: 298 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08026241B2 |
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| 출처 데이터셋 | uspto-grants-2011_09 |
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| ORD ID | ord-525e89e0db04423b8ae69121722b1efc |
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| 출처 메모 | uspto-grants-2011_09 |
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