反应详情

5-Bromo-4-methylpyrimidine (2.90 g, 16.8 mmol) in acetic acid (40 mL) was stirred with bromine (3.18 g, 20.2 mmol) at 80° C. for 40 minutes. After completion of the reaction, the reaction solution was cooled, diluted with ethyl acetate and neutralized with water and 1 M aqueous sodium hydroxide, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=7/1). The resulting product (3.69 g) was dissolved in 60 mL of dimethylformamide and heated with potassium phthalimide (2.84 g, 15.3 mmol) at 80° C. for 1 hour with stirring. After completion of the reaction, the reaction solution was mixed with water and extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform) to give the desired product (4.3 g, 80% yield).

1. customAfter completion of the reaction
2. temperaturethe reaction solution was cooled
3. customthe organic layer was separated
4. dry with materialdried over anhydrous magnesium sulfate
5. customevaporated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=7/1)
7. dissolutionThe resulting product (3.69 g) was dissolved in 60 mL of dimethylformamide
8. customAfter completion of the reaction
9. extractionextracted with chloroform
10. dry with materialthe extract was dried over anhydrous magnesium sulfate
11. customevaporated under reduced pressure
12. customThe resulting residue was purified by silica gel column chromatography (chloroform)