関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Bupropion | HCID 444 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Bupropion Hydrobromide | HCID 11984562 | 74.8% |
反応手順
A 250 ml flask equipped with overhead stirrer and gas inlet was charged with 34 g of bupropion base and 138 ml of isopropanol. The solution was maintained under stirring while 13 g of gaseous HBr was introduced through the gas inlet in a time of 20′ while the internal temperature of the mixture raises from 25 to 40° C. During the gas addition a heavy white precipitate formed. At the end of the gas addition the temperature of the mixture was raised to reflux (80° C.), to get complete solution of the suspended solid. The temperature was then lowered to 25° C. in 1 hour and further lowered to 0-5° C. in 1 additional hour. The precipitate obtained was filtered and washed with 20 ml of cold isopropanol. The discharged wet solid was dried under vacuum (30 mmHg) in a static drier at 50° C. for 16 hours. 34 g of bupropion hydrobromide form I were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07563823B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-e1e11355078b4eb996a3cf06abc8ad24 |
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| 出典メモ | uspto-grants-2009_07 |
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