反应详情

2-Mercapto-1-methyl-2′-phenyl-1H-[4,4′]bipyrimidinyl-6-one (2.76 g, 9.33 mmol) in 1,2-dichloroethane (20 ml) and N-methylpyrrolidone (2 ml) was added to a solution of phosphorus oxychloride (3.83 g, 25.0 mmol) and N-methylpyrrolidone (5.22 g, 52.7 mmol) at 50° C. and the mixture was stirred for 20 minutes. The solution was poured into warm water, and sodium bicarbonate (10.2 g, 121 mmol) was added to the solution and the mixture was stirred until no gas was generated. The resulting solution was partitioned between water and dichloromethane, and the organic layer was washed with water and brine and passed through Celite. The solvent was removed under reduced pressure, and the residue was purified with silica gel column chromatography (eluent; hexane/ethyl acetate=2/1 to 1/1) to afford 2-chloro-1-methyl-2′-phenyl-1H-[4,4′]bipyrimidinyl-6-one (2.08 g, 75%).

1. additionThe solution was poured
2. additionwas added to the solution
3. stirringthe mixture was stirred until no gas
4. customThe resulting solution was partitioned between water and dichloromethane
5. washthe organic layer was washed with water and brine
6. customThe solvent was removed under reduced pressure
7. customthe residue was purified with silica gel column chromatography (eluent; hexane/ethyl acetate=2/1 to 1/1)