反応 #1483122

反応方程式

potassium carbonate

9-(2-formylphenyl)phenanthrene

→

benzo[g]chrysene

収率 44.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.STIRRINGStirring
2. 2
   workup.ADDITIONwas added
3. 3
   その他An aqueous phase was removed
4. 4
   その他an organic phase which had been separated
5. 5
   洗浄was washed with water and saturated brine
6. 6
   乾燥dried with magnesium sulfate
7. 7
   ろ過After the magnesium sulfate was filtered out
8. 8
   濃縮the organic phase was concentrated
9. 9
   その他The resulting residue was purified by means of silica gel column chromatography

実験手順

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.

出典