関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isobutyl iodide | HCID 10556 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione | HCID 96141 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Chloro-1-isobutyl-3-methylpyrimidine-2,4(1H,3H)-dione | HCID 5282566 | 52% |
反応手順
A mixture of 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione (3 g, 18.8 mmol), isobutyl iodide (5 mL, 43.5 mmol) and potassium carbonate (5.3 g, 38.4 mmol) in anhydrous DMF (200 mL) is heated at 50° C. for 8 hours. Additional isobutyl iodide (4.3 mL, 37.5 mmol) is added, and the reaction mixture heated at 50° C. for 24 hours. After hot filtration, the filtrate is evaporated to dryness under reduced pressure. The obtained oil is further purified by silica-gel flash chromatography to give 2.1 g of pure product (Yield: 52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846693B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-a010378496ce4d479c7bed4cc77af8c5 |
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| 出典メモ | uspto-grants-2014_09 |
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