反应详情

温度

80 °C

In DMF, 0.0971 g (0.159 mmols) of 2,5-diiodo-3,4-bis(diethoxyphosphoryl)thiophene and 0.0346 g (0.349 mmols) of commercially available copper(I) chloride were dissolved, to which 0.1744 g (0.383 mmols) of tributylstannylbithiophene was added at room temperature. Thereafter, the reaction mixture was heated to 80° C. and stirred for 12 hours. After the reaction, the reaction mixture was cooled down to room temperature, to which a 0.6 M hydrochloric acid aqueous solution was added, followed by extraction of the resulting product 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) to obtain the specified substance 1. The results are shown in Table 12.

1. additionwas added at room temperature
2. customAfter the reaction
3. additionwas added
4. extractionfollowed by extraction of the resulting product with ethyl acetate
5. washThe organic phase was washed with a saturated saline solution
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was removed
8. distillationby distilling off under reduced pressure
9. customthe resulting product was purified with a silica gel column (ethyl acetate:methanol=15:1)
10. customto obtain the specified substance 1