참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Fluorobenzene | HCID 10008 | — |
| 반응물 | 1-Acetylpiperidine-4-carbonyl chloride | HCID 100950 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 생성물 | 1-Acetyl-4-(4-fluorobenzoyl)piperidine | HCID 117257 | 80% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04886794 |
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| 출처 데이터셋 | uspto-grants-1989_12 |
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| ORD ID | ord-79ff20058e874daeb6a8df84bce5fc68 |
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| 출처 메모 | uspto-grants-1989_12 |
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