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 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | HCID 178527720 | HCID 178527720 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Chloro-6-(methylthio)pyridazine | HCID 252475 | 94% |
反応手順
6-Chloropyridazine-3-thiol (500 mg, 3.41 mmol) synthesized in Example (118a) was dissolved in methanol (20 mL), and sodium methoxide (203 mg, 3.75 mmol) and iodomethane (234 mL, 3.75 mmol) were added, followed by stirring at 60° C. for 30 minutes under nitrogen atmosphere. The reaction solution was cooled to room temperature, water (50 mL) was added, and extraction was carried out twice with ethyl acetate (50 mL). The organic layer was washed with saturated brine, and subsequently dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified using silica gel column chromatography (elution solvent: ethyl acetate/hexane=10%-50%) to afford the desired compound (515 mg, yield 94%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08017610B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-d12603639139418ea143773d750df689 |
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| 出典メモ | uspto-grants-2011_09 |
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