反应详情

温度

0 °C

To a suspension of 2,4-Bis(methyloxy)-5-pyrimidinecarboxylic acid (Prep31, 1.000 g, 5.43 mmol) in N,N-Dimethylformamide (DMF) (35 mL) at 0° C. N,N′-Carbonyldiimidazole (1.321 g, 8.15 mmol) was added and the mixture was stirred for 1 hour at 0° C., then left stirring at rt. After 4 h Triethylamine (2.271 mL, 16.29 mmol) and N,N′-Carbonyldiimidazole (1.321 g, 8.15 mmol), were added to the white suspension. After other 4 h, N,N′-Carbonyldiimidazole (1.321 g, 8.15 mmol) of another batch was added to the suspension. The reaction was left overnight at rt. The solution was then concentrated in vacuo and methanol was added. The solution was stirred at reflux for 2 h. Then the mixture was evaporated in vacuo, the residue was dissolved in DCM and washed with NaHCO3 sat. sol. and then with H2O. Organic phase was dried with Na2SO4 anhydrous, filtered and evaporated in vacuo to obtain 550 mg of the title compound, which was used in the following step without further purification.

1. waitleft
2. stirringstirring at rt
3. additionwere added to the white suspension
4. waitAfter other 4 h
5. waitThe reaction was left overnight at rt
6. concentrationThe solution was then concentrated in vacuo and methanol
7. additionwas added
8. stirringThe solution was stirred
9. temperatureat reflux for 2 h
10. customThen the mixture was evaporated in vacuo
11. dissolutionthe residue was dissolved in DCM
12. washwashed with NaHCO3 sat. sol.
13. dry with materialOrganic phase was dried with Na2SO4 anhydrous
14. filtrationfiltered
15. customevaporated in vacuo