Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Benzyl Alcohol | HCID 244 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2,3-Difluorobenzonitrile | HCID 88935 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3-Fluoro-2-(phenylmethoxy)benzonitrile | HCID 57705211 | — |
Reaktionsschritte
Benzyl alcohol (5.51 mL) was added dropwise over 20 min to a stirred suspension of sodium hydride (2.128 g of a 60% dispersion in mineral oil) and 2,3-difluorobenzonitrile (7.4 g) in THF (100 mL) with external ice bath cooling to maintain temperature around 25° C. After addition was complete, the reaction mixture was stirred at room temperature for 24 h, quenched with water (200 mL) and extracted into ethyl acetate (3×120 mL), combined organics were dried (MgSO4) and evaporated. The residual oil was purified (SiO2 chromatography eluting with 20% ether in isohexane) to give the subtitle compound as an oil (9.70 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08889692B2 |
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| Quelldatensatz | uspto-grants-2014_11 |
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| ORD ID | ord-f120ff53d87e4cdfb8c54600fef750b8 |
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| Quellennotiz | uspto-grants-2014_11 |
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