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Methyl vinyl ketone → 4-[4-(6,11-Dihydrodibenzo[b,e]thiepin-11-ylidene)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 | Piperidine, 4-(dibenzo(b,e)thiepin-6(11H)-ylidene)-1-methyl-, hydrochloride | HCID 121108 | — |
| 反応物 | Fumarate | HCID 5460307 | — |
| 反応物 | 4-dibenzo[b,e]thiepin-11(6H)-ylidenepiperidine | HCID 15077940 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-[4-(6,11-Dihydrodibenzo[b,e]thiepin-11-ylidene)piperidino]-2-butanone | HCID 20371484 | — |
反応手順
A solution of 2.8 g of methylvinylketone in 5 cc of ethanol is added dropwise within 2 minutes to a solution of 7.8 g of 4-(6,11-dihydrodibenzo[b,e]thiepin-11-ylidene)piperidine [M.P. of the fumarate 245°-247°, produced in a manner analogous to that described in Example 9(a), from 4-(6,11-dihydrodibenzo[b,e]thiepin-11-ylidene)-1-methylpiperidine] in 25 cc of ethanol. The reaction mixture is heated at reflux for 1 hour, is then completely concentrated at reduced pressure, and the oily residue, the title compound, is converted into the hydrogen fumarate form. M.P. 180°-182° (decomp.) from ethanol.
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-1bf072ad69b042298bd4f8781556ed18 |
| 出典メモ | uspto-grants-1978_02 |