化工社化工社 化学情報印刷レポート · 研究参考用
Ephedrine → DL-Ephedrine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ephedrine | HCID 9294 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | DL-Ephedrine | HCID 5032 | — |
反応手順
A mixture of d,l-3-[(3,5-dimethoxy-N-ethoxycarbonyl)anilino]butyric acid (136.6 g., 0.44 mole) and l-ephedrine (72.5 g., 0.44 mole) is dissolved in methylene chloride (500 ml.). The methylene chloride is then removed in vacuo to yield the 1-ephedrine salt of d,l-3-[(3,5-dimethoxy-N-ethoxycarbonyl)anilino]butyric acid as an oil, [α]D25 =-20.0 (c=1.0, CHCl3). Addition of ether (1500 ml.) causes crystallization of a white solid which is separated by filtration and dried (102 g.), m.p. 114°-116° C. Recrystallization from ethyl acetate/hexane (1:1) affords 71.1 g. (34%) of the l-ephedrine salt of l-3-[(3,5-dimethoxy-N-ethoxycarbonyl)anilino]butyric acid; m.p. 126°-127° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04400385 |
| 出典データセット | uspto-grants-1983_08 |
| ORD ID | ord-3e5151f4fab7408e8fd9789878c322b7 |
| 出典メモ | uspto-grants-1983_08 |