反应详情

To a solution of 3-[5-chloro-4-(2,4-difluoro-benzyloxy)-2-methyl-6-oxo-6H-pyrimidin-1-yl]-4-methyl-benzoic acid from Step B (230 mg, 0.53 mmol) in tetrahydrofuran (2 mL) was added 1,1′-carbonyldiimidazole (128 mg, 0.79 mmol). After stirring at ambient temperature for three hours, N,N-dimethylhydroxylamine HCl (76 mg, 0.79 mmol) and triethylamine (0.15 mL, 1.06 mmol) were added. The solution continued to stir for eighteen hours. The solution was partitioned between ethyl acetate and water. The organic layer was washed with saturated sodium bicarbonate, water, 5% citric acid and brine and dried over magnesium sulfate. The slurry was filtered and concentrated to provide the amide as a light green oil (160 mg, 65%). MS (M+H): 464

1. stirringto stir for eighteen hours
2. customThe solution was partitioned between ethyl acetate and water
3. washThe organic layer was washed with saturated sodium bicarbonate, water, 5% citric acid and brine
4. dry with materialdried over magnesium sulfate
5. filtrationThe slurry was filtered
6. concentrationconcentrated