Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | Ethyl 7-hydroxychromane-2-carboxylate | HCID 11085381 | — |
| Edukt | 3-Bromopropyl 2-chloro-4-(2,2,2-trifluoroethoxy)phenyl ether | HCID 22737354 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 22737360 | HCID 22737360 | 81,1% |
Reaktionsschritte
To a 40 ml DMF solution of ethyl 7-hydroxy-chromane-2-carboxylate (1.81 g, 8.15 mmol) and 3-bromopropyl 2-chloro-4-(2,2,2-trifluoroethoxy)phenyl ether (3.4 g, 9.8 mmol) was added cesium carbonate (3.2 g, 9.8 mmol). The resulting suspension was heated to 70° C. for 5 hr. The solvent was removed under reduced pressure. The residue was diluted with AcOEt and 2N hydrochloric acid. The organic layer was separated, and the aqueous layer was extracted twice with AcOEt. The combined organic layers were dried over anhydrous Na2SO4, filtered, concentrated, and chromatographed on slica gel eluting with 20% AcOEt/hexanes to give the title compound 3.23 g (81%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06713508B2 |
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| Quelldatensatz | uspto-grants-2004_03 |
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| ORD ID | ord-c41b1a77a6704e59a2c298e1a3132e1f |
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| Quellennotiz | uspto-grants-2004_03 |
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