関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-2-methylpropane | HCID 6555 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-(3-fluoro-4-methylphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one | HCID 21991475 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(3-fluoro-4-methylphenyl)-2-isobutyl-4-methoxycarbonyl-2H-pyridazin-3-one | HCID 21991492 | 85% |
反応手順
To a solution of 6-(3-fluoro-4-methylphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one (5.28 g, 20.0 mmol) in N,N-dimethylformamide (40 mL) were added potassium carbonate (5.53 g, 40.0 mmol) and isobutyl bromide (3.29 g, 24.0 mmol), and the mixture was stirred at 80° C. for 1 hour. The temperature of the reaction mixture was allowed to drop back to room temperature. A saturated aqueous solution of sodium hydrogencarbonate was added, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel [silica gel 100 g, chloroform/methanol (100/1→50/1)) to yield the title compound as an orange oil (5.41 g, 84.9%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087606B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-447057a76e4c472e8ee185e270a27f68 |
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| 出典メモ | uspto-grants-2006_08 |
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