反应详情

Commercially available n-butyl lithium (2.6 M hexane solution, 21.0 mmols) was slowly dropped in a THF solution cooled to −78° C., of 2.14 g (21.0 mmols) of commercially available diisopropylamine. After stirring for 1 hour, a THF solution of 3.00 g (8.41 mmols) of 3,4-bis(diethoxyphosphoryl)thiophene obtained in Example 1 was added. After stirring for further 1 hour at a standing temperature, 8.20 g (25.2 mmols) of commercially available tributylstannyl chloride was dropped, followed by stirring for 4 hours. After completion of the reaction, a disodium hydrogen phosphate/sodium dihydrogen phosphate buffer solution, adjusted to pH=7, was added so as to complete the reaction, followed by extraction with ethyl acetate. The organic phase was washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed, and the resulting crude product was purified with a silica gel column (ethyl acetate) to obtain the specified substance in the form of a transparent oil at a yield of 5.58 g (yield: 100%).

1. additionwas dropped
2. stirringby stirring for 4 hours
3. customAfter completion of the reaction
4. additionwas added so as
5. customthe reaction
6. extractionfollowed by extraction with ethyl acetate
7. washThe organic phase was washed with a saturated saline solution
8. dry with materialdried over anhydrous sodium sulfate
9. customThe solvent was removed
10. customthe resulting crude product was purified with a silica gel column (ethyl acetate)
11. customto obtain the specified substance in the form of a transparent oil at a yield of 5.58 g (yield: 100%)