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With N-Bromosuccinimide; acetic anhydride; at 100℃; for 5.16h;
B. Preparation of 5-bromo-<strong>[5270-94-0]4,6-dimethoxypyrimidine</strong> To the solution of <strong>[5270-94-0]4,6-dimethoxypyrimidine</strong> (5 g, 35.7 mmol) in HOAc (20 mL) at room temperature under argon was added Ac2O (4.6 g, 44.6 mmol). The resulting solution was heated at 100 C. for 10 min and then NBS (7.9 g, 44.6 mmol) was added. Heating was continued at 100 C. for 5 h. Analysis by HPLC/MS indicated that the reaction was complete. After the reaction mixture was cooled to room temperature, water (50 mL) was added. The resulting precipitate was collected by filtration and further washed with water (15 mL*3), then dried under vacuum. The title compound (7.5 g) was obtained as a white solid. 1H NMR (CDCl3): delta 4.05 (s, 6H), 8.32 (s, 1H). 13C NMR (CDCl3): delta 55.2, 89.0, 154.9, 166.8.
To AY-1 (1.25 g, 5.49 mmol)In anhydrous MeOH (15 mL)NaOMe (2.37 g, 43.89 mmol) was added to the solution.The mixture was stirred at rt for 1 h. The solution was filtered and concentrated.The residue was purified by flash chromatography on SiO2 to give Intermediate AY.
With methanol; at 20℃; for 1h;
To a solution of AY-1 (1.25g, 5.49 mmol) in anhydrous MeOH (15 mL) is added NaOMe (2.37g, 43.89 mmol). The mixture is stirred at rt for 1 h. The solution is filtered and concentrated. The residue is purified by Si02 flash chromatography to yield intermediate AY. MS (ES+): m/z 218.9 [M+H]+.
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