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1-Trifluoroacetyl-piperidine-4-carboxylic acid [2-(3-methoxy-phenyl)-ethyl]-amide → 2,2,2-Trifluoro-1-[4-(6-methoxy-3,4-dihydro-isoquinolin-1-yl)-piperidin-1-yl]-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Trifluoroacetyl-piperidine-4-carboxylic acid [2-(3-methoxy-phenyl)-ethyl]-amide | HCID 86583958 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | 2,2,2-Trifluoro-1-[4-(6-methoxy-3,4-dihydro-isoquinolin-1-yl)-piperidin-1-yl]-ethanone | HCID 18172393 | 88.3% |
反応手順
A stirred solution of 1-trifluoroacetyl-piperidine-4-carboxylic acid [2-(3-methoxy-phenyl)-ethyl]-amide (1.04 g, 2.9 mmol) in POCl3 under an atmosphere of N2 was heated at reflux for 2.5 hours. The reaction was allowed to cool to RT and the POCl3 was removed in vacuo. The residual oil was suspended in toluene (20 ml) and concentrated in vacuo (this process was repeated twice more), leaving the desired product as a tan colored solid (0.872 g, 2.56 mmol, 88% yield). MS 341 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06608203B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-e2ab688b7a3f4015909250ff6dcb8c4d |
| 出典メモ | uspto-grants-2003_08 |