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HRID 12662作成日:2026年10月26日
Sodium hydride → 1-[3-(tert-Butyl-dimethyl-silanyloxy)-propyl]-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione
https://huagongshe.com/reaction/12662
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (3-Bromopropoxy)(tert-butyl)dimethylsilane | HCID 607486 | — |
| 反応物 | 5-(3-Methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione | HCID 14914592 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[3-(tert-Butyl-dimethyl-silanyloxy)-propyl]-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione | HCID 68691300 | 37% |
反応手順
To a suspension of 5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione (Prep26, 110 mg, 0.52 mmol) in dry DMF (10 mL), 60% NaH (31 mg, 0.78 mmol) was added. The mixture was then heated at 100° C. for 1 hour. (3-bromo-propoxy)-tert-butyl-dimethyl-silane (180 μl, 0.7 mmol) was then added at room temperature and the reaction was stirred overnight. The solvent was evaporated and the crude was partitioned between NaHCO3 and Et2O. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (2-8) to give the title compound as a white solid (73 mg, 37% 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-02bf8d507037412cb69175d867be4cb6 |
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| 出典メモ | uspto-grants-2010_06 |
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