反应详情

At room temperature, 0.1129 g (0.2 mmols) of 4,3′-bis(diethoxyphosphoryl)-5′-iodo-[2,2′]-bithiophene and 0.0092 g (0.008 mmols) of commercially available tetrakistriphenylphosphine palladium were dissolved in 2 ml of toluene, to which 0.1018 g (0.2 mmols) of 2-(tributylstannyl)-3-(diethoxyphosphoryl)thiophene and 0.0036 g (0.04 mmols) of commercially available copper(I) cyanide were added at room temperature. Thereafter, the reaction mixture was heated and stirred under reflux for 2.5 hours. After the reaction, the reaction mixture was cooled down to room temperature, to which a potassium fluoride aqueous solution added, followed by stirring for 1 hour. The resulting solid was removed by celite filtration and the filtrate was extracted with ethyl acetate. The organic phase was washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed by distilling off under reduced pressure, and the resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane=1:2 and ethyl acetate:hexane=1:1) to obtain the specified substance in the form of a yellow oil at a yield of 0.0919 g (yield: 70%).

1. additionwere added at room temperature
2. temperatureThereafter, the reaction mixture was heated
3. temperatureunder reflux for 2.5 hours
4. customAfter the reaction
5. additionadded
6. stirringby stirring for 1 hour
7. customThe resulting solid was removed by celite filtration
8. extractionthe filtrate was extracted with ethyl acetate
9. washThe organic phase was washed with a saturated saline solution
10. dry with materialdried over anhydrous sodium sulfate
11. customThe solvent was removed
12. distillationby distilling off under reduced pressure
13. customthe resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane=1:2 and ethyl acetate:hexane=1:1)
14. customto obtain the specified substance in the form of a yellow oil at a yield of 0.0919 g (yield: 70%)