化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 1-Cyclohexyl-4-dimethylamino-2-phenyl-2-buten-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | p-Chlorothiophenol | HCID 7815 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3-(Dimethylamino)-1-phenyl-2-propen-1-one | HCID 353460 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-Cyclohexyl-4-dimethylamino-2-phenyl-2-buten-1-ol | HCID 53845847 | — |
反応手順
By using a method similar to that described in Example 35, but starting from 3-dimethylaminoacrylophenone (5 g), phosphorus oxychloride (2.5 cc), p-chlorothiophenol (4.13 g) and sodium cyanoborohydride (1 g), and after evaporating the reaction mixture under reduced pressure (2.7 kPa) at 40° C., a residue is obtained, which is dissolved in ethanol (50 cc). A 3N solution (12 cc) of hydrochloric acid gas in ethyl ether is added to this solution. The precipitate formed is separated off by filtration and then recrystallised from ethanol (70 cc). In this way 3-(4-chlorophenylthio)-1-dimethylamino-3-phenylthio-2-propene (Z) hydrochloride (3.4 g) is obtained in the form of a white powder melting at 226° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04755599 |
| 出典データセット | uspto-grants-1988_07 |
| ORD ID | ord-89680fd193a64abe9bc773ae75999074 |
| 出典メモ | uspto-grants-1988_07 |