関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl mercaptan | HCID 7509 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Bromo-4-methylpyridine | HCID 2734087 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(Benzylthio)-4-methylpyridine | HCID 58349836 | 56% |
反応手順
To a suspension of sodium hydride (60% in oil, 512 mg) in tetrahydrofuran (45 mL) was added dropwise phenylmethanethiol (1.52 g) at room temperature, 2-bromo-4-methylpyridine (2.0 g) was added, and the mixture was stirred at 60° C. for 72 hr. The reaction mixture was diluted with water and extracted twice with ethyl acetate. Combined organic layers were washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent:hexane→hexane-ethyl acetate=24:1) to give the title compound as a brown oil (yield 1.40 g, 56%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08969387B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-22845b20879149f3b6920dd1312864b0 |
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| 出典メモ | uspto-grants-2015_03 |
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