関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2,5-Dichloronitrobenzene | HCID 6977 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(4-Chloro-2-nitrophenyl)piperidine | HCID 285318 | 96.4% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07569536B2 |
|---|
| 出典データセット | uspto-grants-2009_08 |
|---|
| ORD ID | ord-f4280a94034f43cdab6af48d5d2fa757 |
|---|
| 出典メモ | uspto-grants-2009_08 |
|---|