反应详情

A mixture of 5,6-dichloro-3-propyl-1-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]pyrimidine-2,4(1H,3H)-dione (0.22 g), sec-butylmercaptan (0.04 g) and potassium carbonate (0.09 g) in acetonitrile (5 ml) was heated under reflux for 4 hours. The reaction mixture was concentrated to dryness. The resulting residue was dissolved in methanol (15 ml) and 1N hydrochloric acid (1.5 ml) and the mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated to dryness and then the 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 (90 mg, 56%).

1. temperaturewas heated
2. temperatureunder reflux for 4 hours
3. concentrationThe reaction mixture was concentrated to dryness
4. dissolutionThe resulting residue was dissolved in methanol (15 ml)
5. concentrationThe reaction mixture was concentrated to dryness
6. extractionthe residue was extracted with methylene chloride-water
7. washThe organic layer was washed with water
8. customdried
9. customevaporated to dryness
10. customThe resulting residue was purified by column chromatography on silica gel