反应详情

温度

70 °C

3,4-bis(diethoxyphosphoryl)-2,5-diiodothiophene obtained in Example 7, commercially available tetrakistriphenylphosphine palladium (0.10 equivalent) and copper(I) cyanide (commercial product) in amounts indicated in Table 8 were dissolved in different types of solvents indicated in Table 8, to which 2-tributylstannylthiophene (2.2 equivalents) was added at room temperature. Thereafter, the reaction mixture was heated to 70° C. and stirred for 6 to 20 hours. After the reaction, the reaction mixture was cooled down to room temperature, to which a potassium fluoride aqueous solution was added, followed by stirring for 2 hours. Thereafter, the 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 product was purified with a silica gel column (ethyl acetate:methanol=15:1).

1. dissolutionwere dissolved in different types of solvents
2. additionwas added at room temperature
3. customAfter the reaction
4. additionwas added
5. stirringby stirring for 2 hours
6. customThereafter, the solid was removed by celite filtration
7. extractionthe filtrate was extracted with ethyl acetate
8. washThe organic phase was washed with a saturated saline solution
9. dry with materialdried over anhydrous sodium sulfate
10. customThe solvent was removed
11. distillationby distilling off under reduced pressure
12. customthe resulting product was purified with a silica gel column (ethyl acetate:methanol=15:1)