反应详情

To 2-{[5-amino-1-methyl-4-(4-methylphenyl)-1H-pyrazol-3-yl]oxy}ethyl acetate (Preparation 5) (100 mg) in dichloromethane (3 ml) at room temperature was added 4-tert-butylbenzenesulfonylchloride (88 mg), tetrabutylammonium hydrogen sulfate (14 mg) and potassium hydroxide (42 mg), the mixture was sonicated for 3 hrs. The reaction was diluted with water (10 ml) and extracted with ethyl acetate (10 ml). The organic fraction was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (silica, 10 g) eluted with dichloromethane to yield the title compound as a white solid (80 mg).

1. customthe mixture was sonicated for 3 hrs
2. extractionextracted with ethyl acetate (10 ml)
3. dry with materialThe organic fraction was dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography (silica, 10 g)
7. washeluted with dichloromethane