反応 #43682

反応方程式

4-bromobenzo[b]thiophene

styrene

triethylamine

tris(2-methylphenyl)phosphine

→

title compound

4-[(E)-2-Phenylvinyl]benzo[b]thiophene

溶媒

diethyl ether

acetonitrile

反応条件

後処理

1. 1
   温度was refluxed overnight under an argon atmosphere
2. 2
   その他an insoluble material was removed by filtration
3. 3
   洗浄The filtrate washed with 1 mol/L hydrochloric acid, water and brine successively
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他the solvent was removed under reduced pressure
6. 6
   その他The residue was purified by column chromatography on silica gel (eluent: n-hexane-n-hexane/ethyl acetate=5/1)

実験手順

A mixture of 4-bromobenzo[b]thiophene (0.55 g), styrene (0.89 mL), triethylamine (1.81 mL), palladium(II) acetate (59 mg) and tris(2-methylphenyl)phosphine (0.16 g) in acetonitrile (10 mL) was refluxed overnight under an argon atmosphere. The reaction mixture was diluted with diethyl ether and an insoluble material was removed by filtration. The filtrate washed with 1 mol/L hydrochloric acid, water and brine successively, and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane-n-hexane/ethyl acetate=5/1) to give the title compound (0.56 g).

出典