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Hydrochloric Acid → (R)-3-(5-hydroxyhexyl)-1,7-dimethylxanthine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | (R)-3-(5-acetoxyhexyl)-1,7-dimethylxanthine | HCID 54338253 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (R)-3-(5-hydroxyhexyl)-1,7-dimethylxanthine | HCID 11637713 | 85% |
反応手順
To a stirring solution of (R)-3-(5-acetoxyhexyl)-1,7-dimethylxanthine (0.28 g, 0.87 mmol) in methanol (20 ml) was added an anhydrous solution of hydrogen chloride in ethyl ether (1 M, 2.6 ml, 2.6 mmol). After refluxing for 4 hours, the mixture was concentrated under reduced pressure. The residue was treated with saturated aqueous solution of sodium bicarbonate solution (30 ml) and extracted with dichloromethane (3×20 ml). The combined extracts were washed with saturated aqueous sodium chloride solution (30 ml), dried over sodium sulfate and concentrated under reduced pressure to give (R)-3-(5-hydroxyhexyl)-1,7-dimethylxanthine (0.20 g, 85% yield) as a colorless oil that solidified on standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06774130B2 |
| 出典データセット | uspto-grants-2004_08 |
| ORD ID | ord-05a4f91104be4353a2d1edd52020da99 |
| 出典メモ | uspto-grants-2004_08 |