関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tramadol | HCID 33741 | — |
| 反応物 | Naproxen, (-)- | HCID 169118 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (+)-tramadol (R)-naproxen | HCID 131736274 | — |
反応手順
A solution of (R)-naproxen (751 mg, 3.26 mmol) in 4 mL of methanol was added to a solution of (+)-tramadol (430 mg, 1.63 mmol) in 1 mL of methanol. The mixture was stirred for 30 minutes and the solvent was evaporated under vacuum rendering an oil, which solidified by cooling to −197° C. The resulting solid was suspended in 10 mL of diisopropyl ether and stirred for 7 days at room temperature. The resulting suspension was filtered off. The filtrate was washed with 5 mL of diisopropyl ether and dried under vacuum at 40° C. (10 mm Hg) for 16 hours to give a co-crystal of (+)-tramadol-(R)-naproxen in a 1:2 ratio as a crystalline white solid (620 mg, 53%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09393220B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-66ec71c51e90449bbcc928a39446ce0f |
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| 出典メモ | uspto-grants-2016_07 |
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