Potassium Carbonate → HCID 136146568, Verbindung
Reaktionsgleichung
Cl[CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[N:4]=1.[F:15][C:16]1[C:21]([OH:22])=[CH:20][CH:19]=[C:18]([F:23])[C:17]=1[C:24]1[NH:28][C:27](=[O:29])[O:26][N:25]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]2[N:4]=[C:3]([CH2:2][O:22][C:21]3[C:16]([F:15])=[C:17]([C:24]4[NH:28][C:27](=[O:29])[O:26][N:25]=4)[C:18]([F:23])=[CH:19][CH:20]=3)[O:7][N:6]=2)=[CH:9][CH:10]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 25 °C
Versuchsvorschrift
To a solution of 5-chloromethyl-3-(4-chlorophenyl)-[1,2,4]oxadiazole (0.080 g, 0.35 mmol) in anhydrous DMF (2 ml) was added 3-(2,6-difluoro-3-hydroxyphenyl)-4H-[1,2,4]oxadiazol-5-one (0.075 g, 0.35 mmol) and potassium carbonate (0.17 g, 1.22 mmol) was added. The reaction mixture was stirred at 25° C. for 24 h under nitrogen atmosphere. After the completion of the reaction (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure, added water and extracted with EtOAc (3×50 ml). The combined organics was washed with water, dried (Na2SO4), filtered and concentrated. The crude residue was purified over silica (60-120 M) using ethyl acetate/hexane (45:55) as the eluent to provide the title compound as off white solid (0.0088 g, 6%).
Aufarbeitung
- additionwas added
- customAfter the completion of the reaction (TLC monitoring)
- customthe reaction mixture was evaporated to dryness under reduced pressure
- additionadded water
- extractionextracted with EtOAc (3×50 ml)
- washThe combined organics was washed with water
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude residue was purified over silica (60-120 M)
Quellen und Nachweise
- ORD-Eintrag
- ord-3ff973275b42427b97153eb289a95db7
- Quelldatensatz
- uspto-grants-2013_04
- Patentnummer
- US08415383B2
Notizen zur Reaktion
Wird geladen…