反应详情

To 6.1 g (0.03 mol) of the resulting 6-dicyanomethyl-1,3-dimethyluracil was added 1.5 ml of water, and 40 ml of phosphorus oxychloride was added dropwise thereto. After heating the mixture at reflux for 1.5 hours, the phosphorus oxychloride was removed by distillation under normal pressure, and the residue was poured onto ice. The precipitated crystals were collected by filtration. The filtrate was extracted three times with chloroform and dried over anhydrous sodium sulfate. The chloroform was distilled away and the resulting residue was combined with the above obtained crystals. Recrystallization from water-methanol yielded 6.15 g of 6-chloro-1,3-dimethyl-2-oxo-4-dicyanomethylenepyrimidine.

1. additionwas added dropwise
2. temperatureAfter heating the mixture
3. temperatureat reflux for 1.5 hours
4. customthe phosphorus oxychloride was removed by distillation under normal pressure
5. additionthe residue was poured onto ice
6. filtrationThe precipitated crystals were collected by filtration
7. extractionThe filtrate was extracted three times with chloroform
8. dry with materialdried over anhydrous sodium sulfate
9. distillationThe chloroform was distilled away
10. customabove obtained crystals
11. customRecrystallization from water-methanol