化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → (+-)-3,4-Dimethoxyamphetamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Propanone, 1-(3,4-dimethoxyphenyl)- | HCID 69896 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (+-)-3,4-Dimethoxyamphetamine | HCID 8423 | 96.5% |
反応手順
A mixture of 3,4-dimethoxyphenylacetone (51.1 g, 0.26 m) is dissolved in methanol (780 ml), sodium cyanoborohydride (11.3 g, 0.18 m) is added and the mixture is stirred at room temperature for 67 hours. The reaction mixture is adjusted to pH 2 with concentrated HCl and the solvent is evaporated under reduced pressure. The residue is dissolved in H2O (250 ml), the aqueous layer is extracted with ether (3×) and then rendered alkaline with KOH and extracted with CH2Cl2 (3×). After drying, the solvent is evaporated under reduced pressure and the product is distilled at 112°-5°/0.5 mm to yield (VIII) (33.88 g, 67%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04642311 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-9a258557cbe545718551e7d7ba41fd3c |
| 出典メモ | uspto-grants-1987_02 |