反应详情

In a mixed solvent of chloroform and acetic acid at 1:1, 0.0877 g (0.2 mmols) of 4,3′-bis(diethoxyphosphoryl)-[2,2′]-bithiophene was dissolved, to which 0.2250 g (1.0 mmol) of commercially available N-iodosuccinimide was added at room temperature. Thereafter, the reaction mixture was stirred at room temperature for 8 hours. After the reaction, a sodium thiosulfate aqueous solution was added, followed by extraction with chloroform. The organic phase was washed with a 0.2 N sodium hydroxide aqueous 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=2:1) to obtain the specified substance in the form of a yellow solid at a yield of 0.0880 g (yield: 78%). The thus obtained product was used as it is for reaction in Example 12(12).

1. additionwas added at room temperature
2. customAfter the reaction
3. extractionfollowed by extraction with chloroform
4. washThe organic phase was washed with a 0.2 N sodium hydroxide aqueous solution
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was removed
7. distillationby distilling off under reduced pressure
8. customthe resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane=2:1)
9. customto obtain the specified substance in the form of a yellow solid at a yield of 0.0880 g (yield: 78%)
10. customis for reaction in Example 12(12)