Reaktion #1483122

Reaktionsgleichung

potassium carbonate

9-(2-formylphenyl)phenanthrene

→

benzo[g]chrysene

Ausbeute 44.0%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGStirring
2. 2
   workup.ADDITIONwas added
3. 3
   SonstigeAn aqueous phase was removed
4. 4
   Sonstigean organic phase which had been separated
5. 5
   Waschenwas washed with water and saturated brine
6. 6
   Trocknendried with magnesium sulfate
7. 7
   FiltrationAfter the magnesium sulfate was filtered out
8. 8
   Einengenthe organic phase was concentrated
9. 9
   SonstigeThe resulting residue was purified by means of silica gel column chromatography

Vorschrift

24.0 g of the resulting 9-(2-formylphenyl)phenanthrene and 100 mL of dichloromethane were placed in a flask. During stirring at room temperature, 6 drops of methanesulfonic acid were added to the flask by means of a Pasteur pipette. Stirring was conducted at room temperature for further 8 hours. After the completion of the reaction, 100 mL of a 10% aqueous solution of potassium carbonate was added. An aqueous phase was removed and an organic phase which had been separated was washed with water and saturated brine, and then dried with magnesium sulfate. After the magnesium sulfate was filtered out, the organic phase was concentrated. The resulting residue was purified by means of silica gel column chromatography, whereby 5.21 g (yield: 25%) of benzo[g]chrysene was obtained.

Quelle