反应详情

In 5 ml of a mixed solvent of chloroform:acetic acid=1:1, 0.1101 g (0.5 mmols) of 3-(diethoxyphosphoryl)thiophene was dissolved, to which 0.2362 g (1.05 mmols) of commercially available N-iodosuccinimide was added at room temperature. Thereafter, the reaction mixture was stirred at room temperature for 4 days. After the reaction, a disodium hydrogen phosphate/sodium dihydrogen phosphate buffer solution, adjusted to pH=7, was added, followed by extraction with chloroform. The organic phase was washed with a 0.2N sodium hydroxide aqueous solution and dried over anhydrous sodium sulfate. The solvent was removed, and the resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane 1:1) to obtain the specified substance in the form of a yellow oil at a yield of 0.1263 g (yield: 73%). The thus obtained substance was used as it is for reaction in Example 12(9).

1. additionwas added at room temperature
2. customAfter the reaction
3. additionwas added
4. extractionfollowed by extraction with chloroform
5. washThe organic phase was washed with a 0.2N sodium hydroxide aqueous solution
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was removed
8. customthe resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane 1:1)
9. customto obtain the specified substance in the form of a yellow oil at a yield of 0.1263 g (yield: 73%)
10. customis for reaction in Example 12(9)