反应详情

温度

25 °C

To the methanolic (15 mL) solution of (±) ethyl-2-ethoxy-3-[4-[2-ethyl-6-oxo-4-phenyl-1,6-dihydropyrimidin-1-yl]ethoxy]phenyl]propanoate (420 mg, 0.909 mmol) obtained in example 1 was added NaOH (365 mg, 9.125 mmol) in H2O (10 mL), the mixture was stirred at 25° C. for 1 hr, evaporated the solvent under reduced pressure. The residue was added to 50 mL of cold water and washed with ethyl acetate (2×50 mL). The aqueous layer was acidified with 2N HCl and extracted with ethyl acetate (3×100 mL). The combined ethyl acetate layers were washed with water, brine, dried (Na2SO4) and evaporated the solvent, to give a stick compound, which was solidified by either long drying under vacuum or trituration with dry ether to give a white solid (380 mg, 96%) mp: 138-140° C.

1. customevaporated the solvent under reduced pressure
2. additionThe residue was added to 50 mL of cold water
3. washwashed with ethyl acetate (2×50 mL)
4. extractionextracted with ethyl acetate (3×100 mL)
5. washThe combined ethyl acetate layers were washed with water, brine
6. dry with materialdried (Na2SO4)
7. customevaporated the solvent
8. customto give a stick compound, which
9. dry with materialeither long drying under vacuum or trituration with dry ether