反应详情

温度

90 °C

4′-{[4-Ethyl-5-(4-isopropoxyphenyl)-6-oxo-2-propylpyrimidin-1(6H)-yl]methyl}biphenyl-2-carbonitrile (0.5 g) was dissolved in dimethyl sulfoxide (5 mL), and hydroxylamine hydrochloride (0.71 g) and sodium hydrogen carbonate (1 g) were added. The mixture was stirred overnight at 90° C. After cooling, the reaction mixture was diluted with ethyl acetate, washed with water, dried over sodium sulfate and concentrated. The residue was dissolved in tetrahydrofuran (5 mL), and N,N′-carbonyldiimidazole (0.25 g) and 1,8-diazabicyclo[5.4.0]undec-7-ene (0.23 mL) were added. After stirring for 30 min, the reaction mixture was diluted with ethyl acetate, washed with 1 M hydrochloric acid, dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.44 g, 79%).

1. temperatureAfter cooling
2. washwashed with water
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in tetrahydrofuran (5 mL)
6. additionN,N′-carbonyldiimidazole (0.25 g) and 1,8-diazabicyclo[5.4.0]undec-7-ene (0.23 mL) were added
7. stirringAfter stirring for 30 min
8. additionthe reaction mixture was diluted with ethyl acetate
9. washwashed with 1 M hydrochloric acid
10. dry with materialdried over sodium sulfate
11. concentrationconcentrated
12. customThe residue was purified by silica gel column chromatography