関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bazedoxifene Acetate | HCID 154256 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Bazedoxifene | HCID 154257 | 94% |
反応手順
Bazedoxifene acetate (3 g) and dimethylsulfoxide (15 mL) are mixed and heated to 60-70° C. to produce a clear solution, followed by cooling to room temperature and filtration to make it particle free. To the filtrate, toluene (150 mL), 10% aqueous sodium carbonate solution (5 mL) and water (75 mL) are added and the mixture is stirred at room temperature for solid formation. The solid so formed is collected by filtration, washed with toluene (6 mL), water (6 mL) and dried under vacuum below 80° C. for about 7 hours to afford 2.5 g of crystalline bazedoxifene free base Form A.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09212172B2 |
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| 出典データセット | uspto-grants-2015_12 |
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| ORD ID | ord-0616b5f881544275bb673f0cc2cd4451 |
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| 出典メモ | uspto-grants-2015_12 |
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