反应详情

温度

115 °C

A mixture of 1-(2'-cyanobiphenyl-4-yl)methyl-3-propyl-6-propylthiopyrimidine-2,4(1H,3H)-dione (0.77 g), sodium azide (1.8 g) and ammonium chloride (1.48 g) in dimethylformamide (10 ml) was heated at 115° C. for 84 hours. The reaction mixture was diluted with methylene chloride and then the precipitate was filtered. The filtrate was concentrated to dryness in vacuo. The resulting residue was extracted with methylene chloride water. The organic layer was washed with water, dried, and evaporated to dryness. The resulting residue was purified by column chromatography on silica gel to give yellow amorphous powders (0.41 g, 46%).

1. filtrationthe precipitate was filtered
2. concentrationThe filtrate was concentrated to dryness in vacuo
3. extractionThe resulting residue was extracted with methylene chloride water
4. washThe organic layer was washed with water
5. customdried
6. customevaporated to dryness
7. customThe resulting residue was purified by column chromatography on silica gel