反应 #1483122

反应方程式

potassium carbonate

9-(2-formylphenyl)phenanthrene

→

benzo[g]chrysene

收率 44.0%

溶剂

dichloromethane

反应条件

后处理

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

实验过程

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.

来源