反应详情

4-[3-(4-Methoxy-phenyl)-2-oxo-7-phenylamino-3,4-dihydro-2H-pyrimido[4,5-d]pyrimidin-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (70 mg, 0.13 mmol) (from Example 2a supra) was dissolved at 0° C. in a 50% solution of trifluoroacetic acid in dichloromethane (6 mL) that contained 100 μL of water. After stirring for 1.5 hours the mixture was partitioned between ethyl acetate and 1 N aqueous sodium hydroxide and the pH of the aqueous layer was adjusted to 12 by the addition of solid sodium hydroxide. The organic layer was then washed with water, dried over sodium sulfate, filtered and concentrated. The crude material was purified by precipitation out of tetrahydrofuran with excess of pentane to give 3-(4-methoxy-phenyl)-7-phenylamino-1-piperidin-4-yl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one as an off white solid. (Yield 42 mg, 75%).

1. customwas partitioned between ethyl acetate and 1 N aqueous sodium hydroxide
2. additionthe pH of the aqueous layer was adjusted to 12 by the addition of solid sodium hydroxide
3. washThe organic layer was then washed with water
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude material was purified by precipitation out of tetrahydrofuran with excess of pentane