反应详情

温度

70 °C

Into a 100-ml eggplant-shaped flask equipped with a magnetic stirrer and a reflux condenser were added 6.08 g (44 mmol) of potassium carbonate, 4.36 g (20 mmol) of 2-methanesulfonyl-4,6-dimethoxypyrimidine, 3.11 g (22 mmol) of tert-butyl cyanoacetate and 10 ml of N,N-dimethylformamide. The system inside was purged with nitrogen and stirred for 2 hours at 60° C. and for 4 hours at 70° C. The reaction slurry was cooled to room temperature and poured into 30 ml of a 5% aqueous hydrochloric acid solution. Thereto was added 50 ml of water, and concentrated hydrochloric acid was dropped until the system became acidic, followed by sufficient stirring. Then, filtration and washing with 30 ml of water were conducted. The crystals obtained were dried to obtain tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl)acetate as white crystal of 5.4 g. HPLC purity: 99.3% Yield: 97%

1. customInto a 100-ml eggplant-shaped flask equipped with a magnetic stirrer and a reflux condenser
2. customThe system inside was purged with nitrogen
3. temperatureThe reaction slurry was cooled to room temperature
4. additionpoured into 30 ml of a 5% aqueous hydrochloric acid solution
5. additionThereto was added 50 ml of water, and concentrated hydrochloric acid
6. additionwas dropped until the system
7. filtrationThen, filtration
8. washwashing with 30 ml of water
9. customThe crystals obtained
10. customwere dried