関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Methylxanthine | HCID 70639 | — |
| 反応物 | 1-Chloro-5-hydroxy-5-methylhexane | HCID 13747679 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-(5-Hydroxy-5-methylhexyl)-3-methylxanthine | HCID 13747680 | — |
反応手順
83 g (0.5 mol) of 3-methylxanthine are dissolved in 500 ml of 1N sodium hydroxide solution (0.5 mol) under the influence of heat. The mixture is filtered, the water is distilled off under reduced pressure and the sodium salt which remains is dried under a high vacuum. After addition of 1.5 liters of dimethylformamide and 75.3 g (0.5 mol) of 1-chloro-5-hydroxy-5-methylhexane, the mixture is heated at 110° C. for 6 hours, while stirring, filtered hot and evaporated under reduced pressure, the residue obtained is taken up in 1 liter of hot 1N sodium hydroxide solution, the hot solution is filtered and, after cooling to room temperature, 6N hydrochloric acid is added dropwise, with stirring, until a pH of 9 is reached. The precipitate is filtered off with suction, washed neutral and dried in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04833146 |
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| 出典データセット | uspto-grants-1989_05 |
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| ORD ID | ord-bc9497aaf57043adbf80ce262f868ba1 |
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| 出典メモ | uspto-grants-1989_05 |
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