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HRID 1097646作成日:2026年10月26日
Cesium carbonate → 8-chloro-1-(3-hydroxypropyl)-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione
https://huagongshe.com/reaction/1097646
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 3-Bromo-1-propanol | HCID 12308 | — |
| 反応物 | 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59299588 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-chloro-1-(3-hydroxypropyl)-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59395867 | 75% |
反応手順
A solution of 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione (1.0 g, 3.0 mmol) in DMF (15 ml) was treated with caesium carbonate (1.16 g, 3.6 mmol) and 3-bromo-1-propanol (0.3 ml, 3.3 mmol). The mixture was heated at 60° C. for 4 h and then cooled and evaporated. The residue was partitioned between EtOAc (50 ml) and water (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The product was purified by flash chromatography using a gradient elution from cyclohexane to EtOAc. Product-containing fractions were combined and evaporated to give the title compound as a colourless oil (0.82 g, 75%).
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-25feb408d3cd4f77addbaeeb92f4cebe |
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| 出典メモ | uspto-grants-2012_03 |
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