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Triphenylphosphine → 4-[2,2,2-Trifluoro-1-(2-piperidin-1-yl-ethoxy)-1-trifluoromethyl-ethyl]-phenylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 1-(Piperidin-2-yl)ethan-1-ol | HCID 335682 | — |
| 反応物 | 2-(4-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 577801 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-[2,2,2-Trifluoro-1-(2-piperidin-1-yl-ethoxy)-1-trifluoromethyl-ethyl]-phenylamine | HCID 22249326 | — |
反応手順
DEAD (366 mg, 2.1 mmol) was added drop-wise to the solution of 2-(4-aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (520 mg, 2 mmol), 2-piperidylethan-1-ol (260 mg, 2 mmol) and PPh3 (550 mg, 2.1 mmol) in THF (10 mL). The mixture was stirred for 2 h. The reaction was partitioned between EtOAc and aqueous NaHCO3 solution and the organic phase was washed with brine. After concentrated in vacuo, the organic residue was purified by flash chromatography on silica to give the title intermediate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07687643B2 |
| 出典データセット | uspto-grants-2010_03 |
| ORD ID | ord-eaa3025866ad4158889f5a385e1385c4 |
| 出典メモ | uspto-grants-2010_03 |