反应详情

Phosphoeus oxychloride (11.3 g) and N,N-dimethylaniline (3 droplets) were added to ethyl 4-(3-mesityl-2,5-dimethyl-7-oxo-4,7-dihydropyrazolo[1,5-a]pyrimidin-6-yl)butanoate (700 mg, 1.77 mmol), followed by heating under reflux for 1.5 hours. After the reaction, it was treated with ice-water, neutralized with potassium carbonate, extracted with ethyl acetate, dried over anhydrous magnesium sulfate and evaporated. The resulting reaction residue was dissolved in acetonitrile (5 ml) and n-butylamine (2 mL) was added, followed by heating under reflux for six hours. After the reaction, it was treated with water, and then neutralized with potassium carbonate, extracted with ethyl acetate, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (10-25% ethyl acetate/hexane), to give the title compound (2.5 g) as a yellow oil.

1. temperatureby heating
2. temperatureunder reflux for 1.5 hours
3. customAfter the reaction, it
4. extractionextracted with ethyl acetate
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated
7. customThe resulting reaction residue
8. temperatureby heating
9. temperatureunder reflux for six hours
10. customAfter the reaction, it
11. extractionextracted with ethyl acetate
12. dry with materialdried over anhydrous magnesium sulfate
13. customevaporated
14. customThe residue was purified by silica gel column chromatography (10-25% ethyl acetate/hexane)