反应详情

To 4-(tert-butyl)-N-{3-(2-hydroxyethoxy)-1-methyl-4-[4-(trifluoromethyl)phenyl]-1H-pyrazol-5-yl}-N-[(2-methoxyethoxy)methyl]benzenesulfonamide (Preparation 12) in ethanol (1.5 ml) was added hydrochloric acid (6M, 1.5 ml). The reaction mixture was refluxed for 5 hours and then left at room temperature overnight. The reaction was concentrated under reduced pressure and the residue was partitioned between water (10 ml) and ethyl acetate (10 ml). The aqueous was extracted with ethyl acetate (2×20 ml). The organics were combined, dried over magnesium sulfate, filtered and concentrated under reduced pressure to yield the desired product (120 mg) as a white solid. Taken on crude to the next step.

1. temperatureThe reaction mixture was refluxed for 5 hours
2. concentrationThe reaction was concentrated under reduced pressure
3. customthe residue was partitioned between water (10 ml) and ethyl acetate (10 ml)
4. extractionThe aqueous was extracted with ethyl acetate (2×20 ml)
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure