化工社化工社 化学情報印刷レポート · 研究参考用
Doxazosin → Doxazosin Mesylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Doxazosin | HCID 3157 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Doxazosin Mesylate | HCID 62978 | 148% |
反応手順
17.7 g of anhydrous methanesulfonic acid were added to a stirred mixture of 79.0 g of doxazosin and 800 ml of methanol in a 2 1 three-necked round-bottomed flask. During this, the internal temperature rose to 30° C., and a solution formed. After the addition of the methanesulfonic acid was complete, the mixture was stirred for a further 5 h. The resulting precipitate was then filtered off with suction and washed 3× with 50 ml of methanol each time. 141.8 g of moist doxazosin mesylate (modification D) were obtained. This corresponds to 89.2 g of dry substance and a yield of 93.1%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06476033B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-67156bdc60da473a85c0a3f24026ebad |
| 出典メモ | uspto-grants-2002_11 |