참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 2,5-Dichloronitrobenzene | HCID 6977 | — |
| 반응물 | Piperidine | HCID 8082 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(4-Chloro-2-nitrophenyl)piperidine | HCID 285318 | 96.4% |
반응 단계
Piperidine (660 μl, 6.66 mmol, commercially available product) was added at room temperature to an N,N-dimethylformamide (DMF; 1 ml) solution of 1,4-dichloro-2-nitrobenzene (390 mg, 2.03 mmol, commercially available product). The resulting mixture was stirred for 18.5 hours. Water was added to the mixture, and the resulting mixture was extracted three times with ethyl acetate. The obtained organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (30 g, hexane/ethyl acetate=10/1). Thus, 1-(4-chloro-2-nitrophenyl)piperidine (471 mg, 96.4%) was yielded as an orange-colored oily material.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08338362B2 |
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| 출처 데이터셋 | uspto-grants-2012_12 |
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| ORD ID | ord-6caaefe8dfb1402987859e4df68461d6 |
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| 출처 메모 | uspto-grants-2012_12 |
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