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D-Tartaric acid → 17-Cyclobutylmethyl-3-hydroxy-8beta-methylmorphinan-6-one Tartrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | D-Tartaric acid | HCID 439655 | — |
| 反応物 | 17-Cyclobutylmethyl-3-hydroxy-8beta-methylmorphinan-6-one | HCID 53888677 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 17-Cyclobutylmethyl-3-hydroxy-8beta-methylmorphinan-6-one Tartrate | HCID 70528842 | — |
反応手順
To a stirred solution of d-tartaric acid (16.09, 106 mmole) in ethanol (100 ml) was added dropwise a solution of 17-cyclobutylmethyl-3-hydroxy-8β-methylmorphinan-6-one (TR-5130-free base, 32.0 g, 94 mmole) in ethanol (100 ml). After several minutes of stirring, a white solid began to precipitate. The slurry was stirred at room temperature for several hours and then kept in the cold overnight. The solid was collected, washed with cold ethanol followed by ether and dried at atmospheric pressure and 115° C. for one hour to give 32.0 g (69%) of TR-5257 as a white powder, mp. 210°-213° dec.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04259329 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-3082894a3de041108a4101f472094825 |
| 出典メモ | uspto-grants-1981_03 |