反应详情

Methyl 4-[4-(cyclohexylcarbamoyl)-5-propylsulfanyl-pyrazol-1-yl]benzoate (363 mg, 0.94 mmol) (Intermediate #11) was dissolved in methanol (20 mL) and treated at ambient temperature with 2M aqueous sodium hydroxide solution (2.35 mL). The mixture was stirred at ambient temperature for 18 h and then volatiles were removed by evaporation under reduced pressure. The residue was dissolved in water (25 ml) and 2M HCl was added until the pH=4. The mixture was extracted with ethyl acetate (2×25 mL) and the combined extracts were washed with water (2×10 mL) and brine (10 mL), dried (MgSO4) and to evaporated to give the title product as a white solid. (300 mg 85%)

1. customvolatiles were removed by evaporation under reduced pressure
2. dissolutionThe residue was dissolved in water (25 ml)
3. addition2M HCl was added until the pH=4
4. extractionThe mixture was extracted with ethyl acetate (2×25 mL)
5. washthe combined extracts were washed with water (2×10 mL) and brine (10 mL)
6. dry with materialdried (MgSO4)
7. customto evaporated