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Sulfuric Acid → Dimethyl-(2-pyridin-3-yl-cyclohex-2-enylmethyl)amine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Dimethylaminomethyl-1-pyridin-3-yl-cyclohexanol hydrochloride | HCID 69220231 | — |
| 生成物 | Dimethyl-(2-pyridin-3-yl-cyclohex-2-enylmethyl)amine hydrochloride | HCID 69220584 | 57.7% |
反応手順
40 ml 96% strength sulfuric acid were added to 7.8 g dimethylaminomethyl-1-pyridin-3-yl-cyclohexanol hydrochloride, while cooling with ice. When the evolution of gas had ended, the mixture was stirred at room temperature for 45 minutes. The solution was subsequently poured on to approx. 400 g of crushed ice. It was then rendered alkaline by addition of sodium hydroxide lozenges, while cooling with ice, and the mixture was extracted 3× with a total of 600 ml ethyl acetate. The combined organic phases were dried over magnesium sulfate and evaporated to dryness on a rotary evaporator in vacuo at 50° C. 4.2 g dimethyl-(2-pyridin-3-yl-cyclohex-2-enylmethyl)amine hydrochloride were obtained in this way.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07384961B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-aed93a6f05584706a8abf176ef98ba46 |
| 出典メモ | uspto-grants-2008_06 |