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 | Acetone | HCID 180 | — |
| 生成物 | Doxazosin Mesylate | HCID 62978 | — |
反応手順
Doxazosin (100 gms) was charged in acetone (0.8 lit) at room temperature. The contents were stirred for 10 mins at 25-30° C. Methane sulfonic acid (23.2 ml) was charged slowly at 25-30° C. The reaction mass was heated at 35-38° C. and the temperature maintained for 2 hours. The reaction mass was cooled to 25-30° C. and stirred for 1 hour. The solid obtained was filtered and washed with acetone (100 ml). The product was dried at 55-60° C. under vacuum to obtain pure Form IV doxazosin mesylate (115-120 gms) which was characterized by XRD, IR and DSC. Purity according to HPLC: −99.89%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08383627B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-1a6ba6391c4d48a987c1572417db0707 |
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| 出典メモ | uspto-grants-2013_02 |
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