関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Uracil | HCID 1174 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,3-Dioxane, 5-(2-bromoethyl)-2,2-dimethyl- | HCID 178988 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[2-(2,2-Dimethyl-1,3-dioxan-5-yl)ethyl]uracil | HCID 57838979 | 45% |
反応手順
To a solution of uracil (88.5 g, 0.79 mol) in dry DMF (250 mL) was added cesium carbonate (171 g, 0.527 mol) at RT and stirred at the same temperature for 30 min. To the above reaction mixture was added a solution of compound 33 (117 g, 0.527 mol) in dry DMF (250 mL) over a period of 30 min and heated at 50° C. for 24 h. The reaction mixture was filtered, filtrate concentrated under vacuum and crude purified by column chromatography over silica gel (3% methanol in chloroform) to give the title compound (60 g, 45%). TLC: Chloroform/Methanol, 4:1, Rf=0.3
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08017620B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-b0c9446791bd4fca8105e0ad0917d13a |
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| 出典メモ | uspto-grants-2011_09 |
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