関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dexamethasone | HCID 5743 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 131727135 | HCID 131727135 | 82.6% |
反応手順
A 200 mL Erlenmeyer flask equipped with a magnetic stir bar and a rubber septum was charged with 5 grams of dexamethasone (12.7 mmol, 1 equivalent) and 16 mL of anhydrous pyridine. The flask was cooled to 0° C. with an ice bath, and 1.2 mL of methanesulfonyl chloride was added. After 1 hour, 0.8 mL of additional methanesulfonyl chloride was added. At two hours, the solution was poured into 100 mL of cold 1M HCl, forming a precipitate. The precipitate was filtered and redissolved in 250 mL of ethanol, and precipitated into 250 mL of 1M HCl. The precipitate was filtered and recrystallized in ethanol, filtered, and dried under vacuum yielding 4.95 g (82.6%) of dexamethasone mesylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09180132B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-9fb198e288bb401dac4792f81b965445 |
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| 出典メモ | uspto-grants-2015_11 |
|---|