化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-[6-(Acetylamino)pyridin-3-yl]-4-biphenyl-3-ylpiperazine-1-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-Biphenyl-3-yl-piperazine | HCID 2756712 | — |
| 反応物 | 2,2,2-Trichloroethyl[6-(acetylamino)pyridin-3-yl]carbamate | HCID 86245259 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-[6-(Acetylamino)pyridin-3-yl]-4-biphenyl-3-ylpiperazine-1-carboxamide | HCID 16113827 | 18% |
反応手順
A mixed solution of 2,2,2-trichloroethyl[6-(acetylamino)pyridin-3-yl]carbamate (301 mg, 0.923 mmol), 1-biphenyl-3-ylpiperazine (200 mg, 0.839 mmol) and diisopropylethylamine (0.292 ml, 1.68 mmol) in dimethylsulfoxide (2.5 ml) was stirred at 70° C. for 14 hours. To the reaction solution was added water, and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduce pressure. The residue was recrystallized from a mixed solvent of hexane and tetrahydrofuran to give the titled compound (62.6 mg, 18.0%) as solid product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07812025B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-1c9d480f075c46bcae5ed1acf7146185 |
| 出典メモ | uspto-grants-2010_10 |