Reaktionsgleichung
[I:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1.I[CH2:16][CH2:17][CH2:18][CH3:19].CC(C)([O-])C.[K+].O1[CH2:30][CH2:29][CH2:28][CH2:27]1>C(OCC)C.O>[CH2:16]([C:5]1([CH2:27][CH2:28][CH2:29][CH3:30])[C:4]2[CH:3]=[C:2]([I:1])[CH:14]=[CH:13][C:12]=2[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:17][CH2:18][CH3:19]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
Under N2 atmosphere, 0.58 parts of 2-iodo-9H-fluorene, 1.10 parts of 1-iodobutane, and 0.67 parts of potassium tert-butoxide were added into 15 parts of dry tetrahydrofuran, followed by stirring and mixing. Then, the reaction mixture was heated to 50° C. and reacted for 12 hours. After the reaction mixture was cooled, poured the water into the reaction mixture for quenching the reaction, using the diethyl ether to extract the product, and magnesium sulfate was used for dehydration. After removing the solvent, the residual was purified with column chromatography method by using hexane as an eluent, to obtain a compound (32) of the present example. This compound was in a form of a light yellow solid, and the yield of this compound was 94%.
Aufarbeitung
- additionmixing
- customreacted for 12 hours
- temperatureAfter the reaction mixture was cooled
- customfor quenching
- customthe reaction
- extractionto extract the product, and magnesium sulfate
- customAfter removing the solvent
- customthe residual was purified with column chromatography method
Quellen und Nachweise
- ORD-Eintrag
- ord-67fe20fafb014f069195b70da1c871fe
- Quelldatensatz
- uspto-grants-2012_06
- Patentnummer
- US08203068B2
Verknüpfte Notizen
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