반응 #1483122

반응 방정식

potassium carbonate

9-(2-formylphenyl)phenanthrene

→

benzo[g]chrysene

수율 44.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGStirring
2. 2
   workup.ADDITIONwas added
3. 3
   기타An aqueous phase was removed
4. 4
   기타an organic phase which had been separated
5. 5
   세척was washed with water and saturated brine
6. 6
   건조dried with magnesium sulfate
7. 7
   여과After the magnesium sulfate was filtered out
8. 8
   농축the organic phase was concentrated
9. 9
   기타The resulting residue was purified by means of silica gel column chromatography

실험 절차

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.

출처