反应详情

In ethanol, 2.02 g (6.19 mmols) of 2,3-bis(diethoxyphosphoryl)-1,3-butadiene was dissolved, to which 1.63 g (6.81 mmols) of commercially available sodium sulfide nonahydrate was added, followed by stirring at room temperature for 3 days. After completion of the reaction, the reaction mixture was dried over anhydrous sodium sulfate for 1 hour. Ethyl acetate was added to and the resulting mixture was charged into a silica gel column to dissolve out the specified substance with ethyl acetate. Thereafter, the solvent was removed, and the resulting crude product was purified with a silica gel column (ethyl acetate:chloroform=1:2) to obtain the specified substance in the form of a yellow oil at a yield of 1.88 g (yield: 84.3%).

1. additionwas added
2. customAfter completion of the reaction
3. dry with materialthe reaction mixture was dried over anhydrous sodium sulfate for 1 hour
4. additionEthyl acetate was added to and the resulting mixture
5. additionwas charged into a silica gel column
6. dissolutionto dissolve out the specified substance with ethyl acetate
7. customThereafter, the solvent was removed
8. customthe resulting crude product was purified with a silica gel column (ethyl acetate:chloroform=1:2)
9. customto obtain the specified substance in the form of a yellow oil at a yield of 1.88 g (yield: 84.3%)