関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Triacetoxyperiodinane | HCID 159087 | — |
| 反応物 | 1-(4-Hydroxy-butyl)-5-trifluoromethyl-1H-pyrimidine-2,4-dione | HCID 58994224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(5-Trifluoromethyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-yl)-butyraldehyde | HCID 58994197 | 51.7% |
反応手順
1-(4-Hydroxy-butyl)-5-trifluoromethyl-1H-pyrimidine-2,4-dione (Prep 23, 44 mg, 0.17 mmol) was dissolved in dry THF (5 mL), the solution was cooled to 0° C. and Dess-Martin periodinane (127 mg, 0.28 mmol) was added. The mixture was stirred at 0° C. for 1.5 hours. Et2O was added and the solution washed with aqueous saturated NaHCO3. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1) to give 22 mg of the title compound (50% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727988B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-2d9ddf4e5bc948ea8390a84b8afb5556 |
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| 出典メモ | uspto-grants-2010_06 |
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