반응 #3785
ord-a4ed8d077a2e4b55a7f88a3b17be86f8
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후처리
- 1온도the reaction mixture was refluxed for two hours
- 2농축It was then concentrated under reduced pressures
- 3추출extracted with diethylether
- 4세척rinsed with water
- 5기타With the diethylether removed under reduced pressures
- 6기타the product was purified by alumina column chromatogram
실험 절차
1,2-Bis(5-bromo-2-methyl-3-thienyl)hexafluorocyclopentene (1.0 g 0.002 mol) was dissolved in dimethoxyethane (50 ml), and palladium tetra(triphenylphosphine) (120 mg) was added to the mixture which was stirred for 5 minutes under argon atmosphere. With 4-methyl-2-thienyl boric acid (852 mg, 0.006 mol) and an aqueous solution of potassium carbonate (0.1 mol dm-3, 10 ml) were added, the reaction mixture was refluxed for two hours. It was then concentrated under reduced pressures, extracted with diethylether and rinsed with water. With the diethylether removed under reduced pressures, the product was purified by alumina column chromatogram to give 1,2-bis[2-methyl-5-(4-methyl-2-thienyl)-3-thienyl]hexafluorocyclopentene (447 mg, 0.0008 mol).