反応 #577214

反応方程式

m-chlorobenzoic acid

4-allyloxy-4′-cyanobiphenyl

→

4-cyano-4′-glycidylbiphenyl

収率 68.4%

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他obtained
2. 2
   その他Insoluble matters thus deposited were removed by filtration, and water
3. 3
   workup.ADDITIONwas added
4. 4
   その他After separating the mixture
5. 5
   洗浄the organic layer was washed with a saturated aqueous solution of sodium hydrosulfite
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off
8. 8
   その他to obtain a residue, which
9. 9
   その他was purified by silica gel column chromatography
10. 10
    その他subjected to recrystallization from ethanol

実験手順

20 g of m-chlorobenzoic acid was added to a reaction mixture obtained by dissolving 19 g of 4-allyloxy-4′-cyanobiphenyl in 150 mL of methylene chloride as divided into several times, and the mixture was stirred at room temperature for 24 hours. Insoluble matters thus deposited were removed by filtration, and water was added thereto. After separating the mixture, the organic layer was washed with a saturated aqueous solution of sodium hydrosulfite and then dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain a residue, which was purified by silica gel column chromatography and then subjected to recrystallization from ethanol to obtain 13 g of 4-cyano-4′-glycidylbiphenyl.

出典