Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl vinyl ketone → 4-[4-(10,11-Dihydro-5-dibenzo[a,d]-cycloheptenylidene)piperidino]-2-butanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl vinyl ketone | HCID 6570 | — |
| 반응물 | 4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-methylpiperidine | HCID 168897 | — |
| 반응물 | Desloratadine impurity 24 | HCID 1201458 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4-[4-(10,11-Dihydro-5-dibenzo[a,d]-cycloheptenylidene)piperidino]-2-butanone | HCID 20371545 | — |
반응 단계
5.1 g of methylvinylketone are added dropwise at 70° to a solution of 10 g of 4-(10,11-dihydro-5-dibenzo[a,d]cycloheptenylidene)piperidine [M.P. 113°-114°, produced in a manner analogous to that described in Example 4 (a), from 4-(10,11-dihydro-5-dibenzo[a,d]cycloheptenylidene)-1-methylpiperidine] in 100 cc of ethanol, and the mixture is boiled at reflux for 11/2 hours. The reaction mixture is then concentrated by evaporation in a vacuum, the residue is dissolved in acetone, the solution is made acid with hydrogen chloride in ether, is again concentrated by evaporation, and the residue is crystallized first from acetone/ether and then from isopropanol/ether. The hydrochloride of the title compound has an M.P. over 300°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04072756 |
| 출처 데이터셋 | uspto-grants-1978_02 |
| ORD ID | ord-568fc28d2b83448b94f006d634d0637f |
| 출처 메모 | uspto-grants-1978_02 |