反应详情

温度

60 °C

To a solution of 4-methyl-3-[2-methyl-4-(2-methyl-thiazol-4-ylmethoxy)-6-oxo-6H-pyrimidin-1-yl]-benzoic acid methyl ester from Step A, of Example 11 (120 mg, 0.31 mmol) in isopropanol (1.5 mL) was added N-chlorosuccinimide (46 mg, 0.34 mmol) and 2 drops of dichloroacetic acid. The solution was heated at 60° C. for three hours. The solution was allowed to cool and concentrated in vacuo and the residue was partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over magnesium sulfate. The slurry was filtered and concentrated to provide the chlorinated product as colorless oil (125 mg, 96%). MS (M+H): 420

1. temperatureto cool
2. concentrationconcentrated in vacuo
3. customthe residue was partitioned between ethyl acetate and water
4. washThe organic layer was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. filtrationThe slurry was filtered
7. concentrationconcentrated