反应详情

To 25 ml of sulfuric acid was slowly added 8.5 g (0.049 mol) of 6-chloro-1,3-dimethyluracil as prepared in Synthesis Example 1 at 10° to 15° C. To this solution was gradually added 8.5 ml of fuming nitric acid at 0° to 5° C. After stirring for 5 minutes, the reaction mixture was poured onto ice and extracted twice with chloroform. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The resulting crystals were recrystallized from a mixed solvent of ethyl acetate and hexane to give 7.5 g (70%) of 6-chloro-1,3-dimethyl-5-nitrouracil having a melting point of 91° to 92° C.

1. customas prepared in Synthesis Example 1 at 10° to 15° C
2. customat 0° to 5° C
3. additionthe reaction mixture was poured onto ice
4. extractionextracted twice with chloroform
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customThe resulting crystals were recrystallized from a mixed solvent of ethyl acetate and hexane