関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(4-Chloro-2-ethyl-6-fluorobenzofuran-7-yl)-6-trifluoromethyluracil | HCID 23289176 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(4-Chloro-2-ethyl-6-fluorobenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil | HCID 15477208 | 94.5% |
反応手順
0.50 g (1.3 mmol) of 3-(4-chloro-2-ethyl-6-fluorobenzofuran-7-yl)-6-trifluoromethyluracil and 0.30 g (2.3 mmol) of potassium carbonate, were suspended in 20 ml of N,N-dimethylformamide, and 0.23 g (1.6 mmol) of methyl iodide was dropwise added thereto under cooling with ice. After stirring at room temperature for 3 hours, the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed sequentially with water and a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 0.48 g (yield: 92%) of the desired product as white crystals. Melting point: 142-143° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06130187 |
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| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-4cc8c6405c384e7bae5f92be5d72802b |
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| 出典メモ | uspto-grants-2000_10 |
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