関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-Bromo-1,1,1-trifluorobutane | HCID 521006 | — |
| 反応物 | 7-Allyl-8-chloro-1H-purine-2,6(3H,7H)-dione | HCID 59299532 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59299588 | 40% |
反応手順
A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (2.0 g, 8.8 mmol) in DMF (20 ml) was treated with sodium carbonate (1.15 g, 10.8 mmol) and 4-bromo-1,1,1-trifluorobutane (1.86 g, 9.7 mmol). The mixture was stirred at 50° C. for 18 h then cooled and evaporated. The residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The residue was triturated in a mixture of diethyl ether and cyclohexane then the product filtered off and dried to yield the title compound as a white solid (1.18 g, 40%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08143264B2 |
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| 出典データセット | uspto-grants-2012_03 |
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| ORD ID | ord-9da0aabc817a471d9ca88ff34cc418da |
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| 出典メモ | uspto-grants-2012_03 |
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