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Enantholactam → HCID 178443232、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Enantholactam | HCID 12657 | — |
| 反応物 | Dodecylamine | HCID 13583 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | HCID 178443232 | HCID 178443232 | — |
反応手順
To 28.3 g (0.223 mole) of an enantholactam in 250 ml of benzene is added 34.1 g (0.223 mole) of phosphorous oxychloride over 30 minutes. The mixture is stirred at room temperature for 4 hours after which 41.2 g (0.223 mole) of dodecylamine is added. The reaction mixture is stirred at room temperature for 1 hour and refluxed for 4 hours then allowed to stand overnight. The resulting precipitate is washed with benzene, and the benzene wash is extracted with aqueous 2 N hydrochloric acid and combined with the precipitate. The combined fractions are made alkaline with 2N sodium hydroxide, extracted into ether-methylene chloride, dried and recrystallized from isopropyl alcohol to give 2-dodecyliminooctahydroazocine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04061746 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-2b6fff81fdb74047b512baa955c5d4e9 |
| 出典メモ | uspto-grants-1977_12 |