化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → HCID 178483999、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | HCID 178484788 | HCID 178484788 | — |
| 溶媒 | Formaldehyde | HCID 712 | — |
| 溶媒 | Sodium dihydrogen phosphite | HCID 23701735 | — |
| 生成物 | HCID 178483999 | HCID 178483999 | — |
反応手順
To a solution of trans-4-(4-hydroxyphenyl)-N-methylcyclohexanamine, hydrochloride (1.15 g) in dioxane (50 mL), aqueous formaldehyde solution (3.7 mL, 37%) and phosphorous acid monosodium salt (49 mL, 1N) is added concentrated aqueous sodium hydroxide solution until pH is neutral. The solution is stirred at a temperature close to 60° C. for 2 h, cooled to room temperature and brought to pH 7-8 by addition of concentrated aqueous sodium hydroxide solution. Evaporation of dioxane causes precipitation. The precipitate is filtrated and washed with water then diethyl ether to give 1.78 g of trans-N,N-dimethyl-4-(4-hydroxyphenyl)cyclohexanamine as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08076329B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-924767e7af244352b37ea88e4b40b4ab |
| 出典メモ | uspto-grants-2011_12 |