反应详情

温度

-70 °C

Dissolve 50 g (0.26 mol) of 4,6-dichloro-5-nitropyrimidine in 500 mL of CH2Cl2 and cool to -70° C. Add a solution of 24 mL (0.28 mol) dimethylamine, 70 mL (0.40 mol) of diisopropylethylamine, and 100 mL of CH2Cl2 over 30 minutes. Warm to ambient temperature and wash the reaction mixture with 500 mL of 20% K2CO3. Dry the CH2Cl2 portion over MgSO4, treat with charcoal filter, and remove the filtrate under vacuum. Crystallize the residue with ether to provide 4-dimethylamino-6-chloro-5-nitropyrimidine.

1. temperatureWarm to ambient temperature
2. washwash the reaction mixture with 500 mL of 20% K2CO3
3. dry with materialDry the CH2Cl2 portion over MgSO4
4. additiontreat with charcoal
5. filtrationfilter
6. customremove the filtrate under vacuum
7. customCrystallize the residue with ether