反应详情

温度

35 °C

To a solution of ethyl 2-(6-(2,4-dimethoxyphenyl)-4-oxo-2-thioxo-3,4-dihydropyrimidin-1(2H)-yl)acetate (6.8 g, 20.3 mmol) in methanol (34 mL) was added 6N aqueous NaOH (16.9 mL), and the solution was stirred at 35° C. for 3 hours. The mixture was concentrated under reduced pressure, and water (100 mL) was added. The aqueous layer was washed with ethyl acetate (2×200 mL), and acidified with concentrated HCl to pH ˜2. The resultant acidic aqueous solution was extracted with EtOAc (3×200 mL), and the combined organic layers were dried with sodium sulfate, and concentrated under reduced pressure to give the title compound 6.53 g (99%) as a white solid.

1. concentrationThe mixture was concentrated under reduced pressure, and water (100 mL)
2. additionwas added
3. washThe aqueous layer was washed with ethyl acetate (2×200 mL)
4. extractionThe resultant acidic aqueous solution was extracted with EtOAc (3×200 mL)
5. dry with materialthe combined organic layers were dried with sodium sulfate
6. concentrationconcentrated under reduced pressure