Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 4-chloro-1-[4-(4-hydroxy-4-phenyl-1-piperidyl)butyl)-1H-pyrazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1H-Pyrazole, 4-chloro- | HCID 27524 | — |
| 반응물 | 8-Hydroxy-8-phenyl-5-azoniaspiro[4,5]decane | HCID 15837498 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-chloro-1-[4-(4-hydroxy-4-phenyl-1-piperidyl)butyl)-1H-pyrazole | HCID 9840622 | 77.3% |
반응 단계
A mixture of 15.0 g (48 mmol) of 8-hydroxy-8-phenyl-5-azoniaspiro[4,5]decane, 5.4 g (53 mmol) of 4-chloropyrazole and 13.2 g of potassium carbonate in 200 ml of dimethylformamide is heated at reflux for 20 hours. Evaporation to dryness is then carried out at reduced pressure, the residue is redissolved in chloroform and washing is carried out repeatedly with water. The organic phase is dried with anhydrous sodium sulfate and evaporation is carried out at reduced pressure, a crude product being obtained which is suspended in ethyl ether, which is filtered while cold and which is washed with ethyl ether. 12.4 g (37.1 mmol) of 4-chloro-1-[4-(4-hydroxy-4-phenyl-1-piperidyl)butyl]-1H-pyrazole are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05731331 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-0c09083e2b874221ab0a6e445f536398 |
| 출처 메모 | uspto-grants-1998_03 |