Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Thiophenol | HCID 7969 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-(3-Methoxyphenyl)-2-methylpropanal | HCID 13296993 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | HCID 19855338 | HCID 19855338 | — |
Reaktionsschritte
To a solution of 2-(3-methoxyphenyl)-2-methylpropanal (20.0 g, 112 mmoles) in 90 mL of N-methylpyrrolidinone was added thiophenol (11.5 mL, 112 mmoles) and anhydrous K2CO3 (1.55 g, 11.2 mmoles). The mixture was stirred at 210-215 ° C. for 3 h. After cooling, the mixture was partitioned between Et2O and 5% aqueous NaOH. The aqueous layer was acidified with dilute HCl and extracted with DCM. The combined organic extracts were dried over Na2SO4, filtered, and evaporated. Chromatography of the residue using 25% EtOAc—hexane as eluent gave the title compound, 10.3 g, as a pale yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07259266B2 |
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| Quelldatensatz | uspto-grants-2007_08 |
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| ORD ID | ord-a19de66661c4486281a79671dab7af78 |
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| Quellennotiz | uspto-grants-2007_08 |
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