Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Toluene | HCID 1140 | — |
| Edukt | 2-(4-morpholinyl)-8-phenyl-4H-1-benzopyran-4-one | HCID 3973 | — |
| Edukt | Lawesson's reagent | HCID 87949 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 44180853 | HCID 44180853 | 135,1% |
Reaktionsschritte
A 2 mL conical microwave vial was charged with a magnetic stirring bar, 2-morpholino-8-phenyl-4H-chromen-4-one (LY294002) (150 mg, 488 μmol), Lawesson's reagent (118 mg, 293 μmol), and toluene (2 mL). The reaction mixture was sealed, and the reaction mixture was magnetically stirred and heated via microwave irradiation to 130° C. for 20 minutes. The final mixture was poured onto water (approximately 30 mL), extracted with dichloromethane (3×5 mL), the combined extracts dried over anhydrous magnesium sulfate, filtered and concentrated to dryness. Purification via column chromatography (silica gel; hexanes/ethyl acetate (1:1), then 100% ethyl acetate) afforded pure 2-morpholino-8-phenyl-4H-chromene-4-thione (68) (128 mg, 81% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08557807B2 |
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| Quelldatensatz | uspto-grants-2013_10 |
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| ORD ID | ord-ab050b876fc049279c98c58122f878ad |
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| Quellennotiz | uspto-grants-2013_10 |
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