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Methyl vinyl ketone → 4-[4-(10,11-Dihydro-5-dibenzo[a,d]-cycloheptenylidene)piperidino]-2-butanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl vinyl ketone | HCID 6570 | — |
| 反応物 | 4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-methylpiperidine | HCID 168897 | — |
| 反応物 | Desloratadine impurity 24 | HCID 1201458 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-[4-(10,11-Dihydro-5-dibenzo[a,d]-cycloheptenylidene)piperidino]-2-butanone | HCID 20371545 | — |
反応手順
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°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04072756 |
| 出典データセット | uspto-grants-1978_02 |
| ORD ID | ord-568fc28d2b83448b94f006d634d0637f |
| 出典メモ | uspto-grants-1978_02 |