反应详情

To a stirred solution of 5-benzyloxy-2-[1-(2,5-dichlorophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid tert-butyl ester (204) (2.0 g, 3.788 mmol) in tetrahydrofuran-H2O (2:1) (30 mL) Li(OH).H2O (1.591 g, 37.88 mmol) was added, then the reaction mixture was stirred under reflux for 16 h. Silica thin layer chromatography was performed (40% ethyl acetate in hexane, Rf=0.1). After completion of the reaction, volatiles were removed, the reaction mixture was diluted with water, the pH was adjusted to pH ˜7 with 1N HCl, then the reaction mixture was extracted with ethyl acetate. The organic part was dried with Na2SO4, then concentrated to get pure 5-benzyloxy-2-[1-(2,5-dichlorophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid (205) (1.3 g, 72.5%) as a white solid.

1. temperatureunder reflux for 16 h
2. customAfter completion of the reaction, volatiles
3. customwere removed
4. additionthe reaction mixture was diluted with water
5. extractionthe reaction mixture was extracted with ethyl acetate
6. dry with materialThe organic part was dried with Na2SO4
7. concentrationconcentrated