関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Pentanone, 5-bromo- | HCID 77493 | — |
| 反応物 | 4-(9-Xanthenylidene)piperidine | HCID 15780516 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-[4-(9-Xanthenylidene)piperidino]-2-pentanone | HCID 20371528 | — |
反応手順
7.2 g of 5-bromo-2-pentanone in 50 cc of chloroform are added dropwise to a suspension of 10.0 g of 4-(9-xanthenylidene)piperidine [M.P. 147°-149°, produced from N-methyl-4-(9-xanthenylidene)piperidine] and 9.25 g of sodium carbonate in 200 cc of chloroform. The reaction mixture is boiled at reflux for 17 hours, is filtered, concentrated by evaporation, the evaporation residue is placed on a column of 100 g of silica gel and elution is effected with chloroform containing 1% of methanol. The evaporation residue of the eluate is dissolved in acetone and made weakly acid to Congo red with hydrogen chloride in ether. The 5-[4-(9-xanthenylidene)piperidino]-2-pentanone hydrochloride which precipitates immediately is recrystallized from alcohol. M.P. 248°-251° (decomp.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04072756 |
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| 出典データセット | uspto-grants-1978_02 |
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| ORD ID | ord-47ac54bf25334b349e0ffafc2ca17317 |
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| 出典メモ | uspto-grants-1978_02 |
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