化工社化工社 化学情報印刷レポート · 研究参考用
p-Fluorophenethylamine → N-[2-(4-fluoro-phenyl)-ethyl]-4-pentafluoroethyl-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Fluorophenethylamine | HCID 4653 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 反応物 | 4-(1,1,2,2,2-Pentafluoroethyl)benzoic acid | HCID 23067883 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-[2-(4-fluoro-phenyl)-ethyl]-4-pentafluoroethyl-benzamide | HCID 86613992 | 99.3% |
反応手順
A solution of 4-pentafluoroethyl-benzoic acid (500 mg, 2.08 mmol), 2-(4-fluorophenyl)ethylamine (319 mg, 2.29 mmol), 4-methylmorpholine (632 mg, 6.24 mmol), and HBTU (1.19 g, 3.12 mmol) in DMF (38 mL) was stirred at RT for 16 h, then the reaction mixture was partitioned between water and ethyl acetate. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (SiO2, heptane-ethyl acetate gradient) afforded the title compound (746 mg, 99%). White solid, MS (ISP) 362.2 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745477B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-43582dbf12b64768b36d16026bb44d98 |
| 出典メモ | uspto-grants-2010_06 |