反应详情

In 3 ml of anhydrous methanol, 23 mg of sodium metal was dissolved, and to the resulting solution, 180 mg of 6-chloro-4-(1-pyrazolyl)pyrimidine in 2 ml of anhydrous methanol was added dropwise with stirring at room temperature in a stream of nitrogen overnight. The solvent was distilled off under reduced pressure, and the residue was extracted with 20 ml of methylene chloride. The organic layer was washed with 5 ml of saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was distilled away, and a residue was purified by a silica gel column chromatography using chloroform to give an amorphous product. The product was recrystallized from n-hexane to provide 132 mg of the plate crystal 6-methoxy-4-(1-pyrazolyl)pyrimidine having a melting point of 108.5°-109° C.

1. distillationThe solvent was distilled off under reduced pressure
2. extractionthe residue was extracted with 20 ml of methylene chloride
3. washThe organic layer was washed with 5 ml of saturated sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was distilled away
6. customa residue was purified by a silica gel column chromatography
7. customto give an amorphous product
8. customThe product was recrystallized from n-hexane