反应详情

A mixture of 5-cyano-4-hydroxy-2-methylsulfanylpyrimidine (48.33 g) from Example 1 and phosphorus oxychloride (150 mL) was heated at reflux for 3 hours. The reaction mixture was allowed to cool to room temperature, filtered, and the filtrate was concentrated to dryness under vacuum. The residue was partitioned between methylene chloride and ice water. The organic layer was separated, washed with water, dried over magnesium sulfate, filtered, and evaporated under reduced pressure. The residue was heated to reflux in hexane (750 mL) with stirring. The hot hexane solution was decanted from the insoluble material and allowed to cool to room temperature to afford 32 g of the title compound 4-chloro-5-cyano-2-methylsulfanyl-pyrimidine.

1. temperaturewas heated
2. temperatureat reflux for 3 hours
3. filtrationfiltered
4. concentrationthe filtrate was concentrated to dryness under vacuum
5. customThe residue was partitioned between methylene chloride and ice water
6. customThe organic layer was separated
7. washwashed with water
8. dry with materialdried over magnesium sulfate
9. filtrationfiltered
10. customevaporated under reduced pressure
11. temperatureThe residue was heated
12. temperatureto reflux in hexane (750 mL)
13. customThe hot hexane solution was decanted from the insoluble material
14. temperatureto cool to room temperature