反应详情

In a 50 ml flask at low temperature, methyl glycolate (0.22 ml, 2.8 mmol) and sodium hydride (114 mg, 2.8 mmol) were dissolved in N,N-dimethyl formamide (7 ml) and then stirred for 10 minutes. 4,6-dichloro-5-nitro-pyrimidine (500 mg, 2.6 mmol) dissolved in N,N-dimethyl formamide (6.5 ml) was added thereto dropwise and then stirred at the same temperature for additional 10 minutes, and then the temperature was raised to room temperature and stirred for additional 10 hours. After completion of the reaction by adding water, the mixture was extracted with dichloromethane, and the combined organic layer was washed with saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography eluting with a solvent of dichloromethane to obtain yellow liquid (280 mg, 44%).

1. additionwas added
2. stirringdropwise and then stirred at the same temperature for additional 10 minutes
3. stirringstirred for additional 10 hours
4. customAfter completion of the reaction
5. extractionthe mixture was extracted with dichloromethane
6. washthe combined organic layer was washed with saturated saline solution
7. dry with materialdried over anhydrous sodium sulfate (Na2SO4)
8. filtrationfiltered
9. customevaporated under reduced pressure
10. customThe residue was purified by column chromatography
11. washeluting with a solvent of dichloromethane