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4-Fluorobenzoyl chloride → N-(1-benzylpiperidin-4-yl)-4-fluorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Fluorobenzoyl chloride | HCID 67879 | — |
| 反応物 | 1-Benzyl-4-piperidylamine | HCID 415852 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Diisopropylethylamine | HCID 81531 | — |
| 生成物 | N-(1-benzylpiperidin-4-yl)-4-fluorobenzamide | HCID 702501 | 70.6% |
反応手順
To a solution of 1-benzyl-4-aminopiperidine (1.13 g) in dichloromethane (10 ml) were added a solution of 4-fluorobenzoyl chloride (0.99 g) in dichloromethane (1 ml) and diisopropylethylamine (1.09 ml) under cooling on an ice-water bath. The mixture was warmed to ambient temperature slowly under stirring. The mixture was diluted with dichloromethane and washed with water, saturated aqueous sodium hydrogen carbonate, water, and brine. After drying with magnesium sulfate, the solvents were removed under reduced pressure. A residue was purified by column chromatography (silica gel 100 ml, dichloromethane:methanol=15:1). After rinse with diisopropyl ether-n-hexane (1:1), N-(1-benzylpiperidin-4-yl)-4-fluorobenzamide (1.31 g) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06710043B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-2a6f47bbdaae4925b1a064929ab38b76 |
| 出典メモ | uspto-grants-2004_03 |