関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diethylphosphite | HCID 3780918 | — |
| 反応物 | 2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone | HCID 14373045 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-1-(4-(piperidin-1-yl)phenyl)ethanone | HCID 15864546 | 100% |
反応手順
2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone (3 g, 8.3 mmol) (from Step A above) was dissolved in tetrahydrofuran (15 mL), and cooled to 0° C. To the resulting solution were added dropwise diethylphosphite (1.13 mL, 8.7 mmol) and triethylamine (1.21 mL, 8.7 mmol) in tetrahydrofuran (7 mL) at 0° C. with stirring. The mixture was slowly warmed to room temperature and stirred for 6 h. The reaction mixture was concentrated in vacuo and poured into ice/water. The precipitate was collected by filtration, washed with water and dried in vacuo to provide 2-bromo-1-[4-(1-piperidinyl)phenyl]ethanone (2.3 g, 100% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094896B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-ff4256aaf0c04c6c9ceb8c97dc41cecd |
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| 出典メモ | uspto-grants-2006_08 |
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