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Triazabicyclodecene → 4-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-4-oxo-butyric Acid Ethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triazabicyclodecene | HCID 79873 | — |
| 反応物 | 2-Chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone | HCID 11358461 | — |
| 反応物 | 4-(5-Chloro-2-hydroxy-phenyl)-4-oxo-butyric Acid Ethyl Ester | HCID 68447374 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-4-oxo-butyric Acid Ethyl Ester | HCID 68447382 | 45% |
反応手順
A solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.11 g, 0.36 mmol), 4-(5-chloro-2-hydroxy-phenyl)-4-oxo-butyric acid ethyl ester (0.11 g, 0.43 mmol) and 1,5,7-triazabicyclo[4,4,0]dec-5-ene bound to polystyrene crosslinked with 2% DVB (0.21 g, 0.54 mmol) in acetonitrile (1.8 mL) was stirred at ambient temperature for 12 hours. The reaction mixture was filtered through a glass frit, concentrated in vacuo and purified via flash chromatography on silica gel to give the title compound (0.084 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098212B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-fe8e31829e854627b42103dff1a859eb |
| 出典メモ | uspto-grants-2006_08 |