化工社化工社 化学情報印刷レポート · 研究参考用
2,5-Difluoronitrobenzene → 1-Benzyl-4-(4-fluoro-2-nitrophenylamino)-piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Difluoronitrobenzene | HCID 67767 | — |
| 反応物 | 1-Benzyl-4-piperidylamine | HCID 415852 | — |
| 溶媒 | N-Methyl-2-piperidone | HCID 13603 | — |
| 生成物 | 1-Benzyl-4-(4-fluoro-2-nitrophenylamino)-piperidine | HCID 21262765 | 86.9% |
反応手順
2,5-Difluoro-nitrobenzene (21.5 g), 1-benzyl-4-amino-piperidine (52.3 g) and N-methyl-piperidone (100 ml) were stirred at 100° C. for 3 h. After cooling the mixture was partitioned between water and ethyl acetate and the aqueous layer was extracted twice with ethyl acetate. The combined organic layers were extracted 5 times with water, and the solvent was evaporated in vacuo. The target compound was crystallized from methanol to yield 38.7 g of the title compound as orange crystals (mp. 86-87° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07723360B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-fbc85c14669d45c2a00413062a2b87bd |
| 出典メモ | uspto-grants-2010_05 |