Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Benzyl mercaptan | HCID 7509 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2-Bromo-4-methylpyridine | HCID 2734087 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2-(Benzylthio)-4-methylpyridine | HCID 58349836 | 56% |
Reaktionsschritte
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%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08969387B2 |
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| Quelldatensatz | uspto-grants-2015_03 |
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| ORD ID | ord-22845b20879149f3b6920dd1312864b0 |
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| Quellennotiz | uspto-grants-2015_03 |
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