Reaktionsgleichung
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([CH3:11])=[C:7]2[C:3]=1[CH:4]=[CH:5][CH2:6]2.[CH2:12]=O.[C:14]1([CH3:24])[CH:19]=[CH:18][C:17](S(O)(=O)=O)=[CH:16][CH:15]=1.[C:25]1([CH3:31])[CH:30]=CC=C[CH:26]=1>>[CH3:24][C:14]1[CH:19]=[CH:18][C:17]([CH3:12])=[C:16]2[C:15]=1[CH:26]=[C:25]([CH2:31][C:5]1[CH2:4][C:3]3[C:7]([CH:6]=1)=[C:8]([CH3:11])[CH:9]=[CH:10][C:2]=3[CH3:1])[CH2:30]2Komponenten
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
In a 500 mL flask equipped with magnetic stirring bar were introduced 10 g (0.069 moles) of 4,7-dimethyl-indene, 1.04 g (0.035 moles) of formalin and 2.64 g (0.014 moles) of para-toluenesulphonic acid in 100 ml of toluene; the mixture was heated to 80° C. and was maintained under stirring for 3 hours at 80° C. Then the reaction was quenched with water/NaHCO3; the conversion, measured by gas chromatographic analysis, was 82.4%. The organic layer was separated, washed with water and brought to dryness under reduced pressure. The crude product was crystallized upon standing at room temperature, and then was further purified by washing with pentane or MeOH, thus isolating 5.1 g of bis(4,7-dimethyl-2-indenyl)methane (purity of 90.2% by G.C.; yield=44.1%).
Aufarbeitung
- customIn a 500 mL flask equipped with magnetic stirring bar
- temperaturewas maintained
- customThen the reaction was quenched with water/NaHCO3
- customThe organic layer was separated
- washwashed with water
- customThe crude product was crystallized
- customupon standing at room temperature
- customwas further purified
- washby washing with pentane or MeOH
Quellen und Nachweise
- ORD-Eintrag
- ord-b5374acbc004471ead25422deb1580ce
- Quelldatensatz
- uspto-grants-2005_03
- Patentnummer
- US06872863B2
Verknüpfte Notizen
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