참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Doxazosin | HCID 3157 | — |
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | Doxazosin Mesylate | HCID 62978 | 89% |
반응 단계
Doxazosin base (0.277 mol; 125 g) was charged in acetone (1875 ml) and stirred at 25° C. to obtain slurry. On cooling the slurry to 10-15° C., methanesulphonic acid (0.33 mol; 31.96 g) was added to it. The contents were stirred for 10-15 min at 10-15° C. and then stirring continued at 25° C. for 2 hr. The solid obtained was filtered, washed with acetone and dried at 50-55° C. to obtain solid. The solid was purified by refluxing in methanol (1500 ml) for 1 hr. The slurry was cooled to room temperature, filtered, washed with methanol and then dried at 60° C. under reduced pressure to obtain 135 g of pure doxazosin mesylate (HPLC purity −99.81%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08426590B2 |
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| 출처 데이터셋 | uspto-grants-2013_04 |
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| ORD ID | ord-9ce08473a972475283b8c15229ce2a66 |
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| 출처 메모 | uspto-grants-2013_04 |
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