関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | 5,6-Dimethyluracil | HCID 96031 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,5,6-Trimethyluracil | HCID 22223251 | — |
反応手順
6.00 g (42.9 mmol) 5,6-dimethyluracil was dissolved in 26 mL of hexamethyldisilazane and 2.1 mL DMF. The mixture was heated for 11 hours at 150° C. and the excess of hexamethyldisilazane was removed under reduced pressure. Toluene was added to the mixture and evaporated off under reduced pressure to remove any residual hexamethyldisilazane. The residue was dissolved in 25 mL of iodomethane, refluxed for 2 hours, the excess iodomethane then evaporated off under reduced pressure and the residue recrystallized from deionised water yielding after drying 5.76 g (87%) of 1,5,6-trimethyluracil (m.p. 254–257° C., lit. 256–258° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07018786B2 |
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| 出典データセット | uspto-grants-2006_03 |
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| ORD ID | ord-aaa8c976615b4462a9470aef40471c31 |
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| 出典メモ | uspto-grants-2006_03 |
|---|