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Methyl iodide → 8-Bromo-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 8-bromo-3-methyl-3,7-dihydro-1H-purine-2,6-dione | HCID 1548797 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-Bromo-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione | HCID 702242 | 93.4% |
反応手順
To a stirring suspension of 8-bromo-3-methylxanthine (prepared as described above for CT12440) (12.25 g, 50.0 mmol) and potassium carbonate (8.62 g, 62.5 mmol) in dimethylformamide (150 ml) was added methyl iodide (7.81 g, 55.0 mmol). After stirring overnight at room temperature, the mixture was poured into ice cold water (400 ml) and stirred at 0-5° C. for 1 hour. The precipitate was filtered, rinsed with water (5x 25 ml) and dried under vacuum to provide 8-bromo-3,7-dimethylxanthine (12.10 g, 93% yield) as a beige solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06878715B1 |
| 出典データセット | uspto-grants-2005_04 |
| ORD ID | ord-9655b689d12b473bb284ec4c9816e161 |
| 出典メモ | uspto-grants-2005_04 |