반응 #3786

반응 방정식

1,2-bis(5-bromo-2-methyl-3-thienyl)hexafluorocyclopentene

5-(5-trimethylsilyl-2-thienyl)-2-thienyl boric acid

potassium carbonate

→

hexafluorocyclopentene

수율 35.0%

용매

dimethoxyethane

반응 조건

후처리

1. 1
   온도the reaction mixture was refluxed for two hours
2. 2
   농축It was then concentrated under reduced pressures
3. 3
   추출extracted with diethylether
4. 4
   세척rinsed with water
5. 5
   기타With the diethylether removed under reduced pressures
6. 6
   기타the 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 5-(5-trimethylsilyl-2-thienyl)-2-thienyl boric acid (1.4 g, 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{5-trimethylsilyl-2-thienyl)-2-thienyl}-3-thienyl]hexafluorocyclopentene (550 mg, 0.0007 mol).

출처