反应详情

To 2-mercapto-6-hydroxy-4-phenylpyrimidine (10 g) in ‘880’ ammonia solution (100 ml) was carefully added Raney nickel (32.5 g, 50% slurry) portionvise. Immediate effervescence took place. The mixture was heated to reflux for 4 hours, filtered and concentrated under reduced pressure. The initial residue was azeotroped with toluene (×2) to remove final traces of water. The pale blue residue was dissolved in hot ethanol and filtered and then the filtrate was treated with charcoal. The resulting green solution was evaporated under reduced pressure to afford crude 4-hydroxy-6-phenylpyrimidine (4.65 g) as a green solid (m.p.>300° C.) which was used in the next stage without further purification.

1. temperatureThe mixture was heated
2. temperatureto reflux for 4 hours
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe initial residue was azeotroped with toluene (×2)
6. customto remove final traces of water
7. dissolutionThe pale blue residue was dissolved in hot ethanol
8. filtrationfiltered
9. additionthe filtrate was treated with charcoal
10. customThe resulting green solution was evaporated under reduced pressure