関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Fluorobenzene | HCID 10008 | — |
| 反応物 | 1-Acetylpiperidine-4-carbonyl chloride | HCID 100950 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 1-Acetyl-4-(4-fluorobenzoyl)piperidine | HCID 117257 | 80% |
反応手順
The title compound was prepared as disclosed in U.S. Pat. No. 3,576,810 as follows: A mixture of 93 g (0.7 mole) of aluminum chloride in 150 ml of fluorobenzene was stirred while 70 g (0.37 mole) of 1-acetylisonipecotic acid chloride was added in small portions. After the addition was complete, the mixture was refluxed for one hour. The mixture was poured onto ice and the two resulting layers were separated. The aqueous layer was extracted twice with chloroform and the chloroform extracts were added to the fluorobenzene which was separated previously. The organic solution was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and 73.7 g (80%) of 1-acetyl-4-(p-fluorobenzoyl)-piperidine was obtained as a crystalline residue. Recrystallization from ligroin-isopropyl ether gave a white crystalline product melting at 75°-78° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04886794 |
|---|
| 出典データセット | uspto-grants-1989_12 |
|---|
| ORD ID | ord-79ff20058e874daeb6a8df84bce5fc68 |
|---|
| 出典メモ | uspto-grants-1989_12 |
|---|