関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene | HCID 8462 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[2-Nitro-4-(trifluoromethyl)phenyl]piperidine | HCID 2775751 | — |
反応手順
Piperidine (5.50 ml, 55.5 mmol, commercially available product) was added at 0° C. to an N,N-dimethylformamide (DMF; 7 ml) solution of 1-chloro-2-nitro-4-(trifluoromethyl)benzene (5.00 g, 22.4 mmol, commercially available product). The resulting mixture was stirred for 40 minutes. 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 (200 g, hexane/ethyl acetate=8/1). Thus, 1-[2-nitro-4-(trifluoromethyl)phenyl]piperidine (6.13 g, quant.) was yielded as an orange-colored solid.
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-fc6a2541feda478f9210a980a7f0f14e |
|---|
| 出典メモ | uspto-grants-2009_08 |
|---|