反应详情

To 1-methyl-4-(4-methylphenyl)-3-(2-phenoxyethoxy)-1H-pyrazol-5-amine (Preparation 2) (105 mg) in dichloromethane (5 ml) at room temperature was added 4-tert-butylbenzenesulfonylchloride (265 mg), tetrabutylammonium hydrogen sulfate (28 mg) and potassium hydroxide (265 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 (101 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