참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperidine | HCID 8082 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-Chloro-2-nitroaniline | HCID 101068 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-Nitro-3-(piperidin-1-yl)aniline | HCID 12597268 | 70.3% |
반응 단계
To a solution of 3-chloro-2-nitroaniline (CXXI) (2.00 g, 11.6 mmol, 1 eq) and piperidine (2.95 g, 34.7 mmol, 3 eq) in DMF (60 ml) was added K2CO3 (4.78 g, 34.4 mmol, 3 eq) in one portion and the mixture was stirred at 120° C. under nitrogen overnight. The reaction mixture was diluted with ethyl acetate (60 ml) and washed with saturated NaHCO3 solution (50 mL). The organic phases were dried over Na2SO4 and concentrated in vacuo, the resultant residue was purified by silica gel column chromatography (PE:EtOAc=5:1→1:1) to give 2-nitro-3-(piperidin-1-yl)aniline (CXXII) (1.8 g, 8.14 mmol, 70.3% yield) as a black solid. ESIMS found for C11H15N3O2 m/z 222 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08883822B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-7f8b2d13be7047229a65ac2000eb1803 |
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| 출처 메모 | uspto-grants-2014_11 |
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