反应详情

温度

80 °C

A solution of Sodium hydroxide (6.67 mL, 13.34 mmol) was added in one portion to a stirred solution of ethyl 5-tert-butyl-1-(4-chloro-3-(trifluoromethyl)phenyl)-1H-pyrazole-4-carboxylate (Intermediate #120) (1 g, 2.67 mmol) in methanol (20 mL). The resulting suspension was stirred at 80° C. for 6 hours. The resulting mixture was evaporated to remove the methanol, washed with ether (20 mL). The reaction mixture was acidified with 2M HCl, extracted with ethyl acetate (2×30 mL) The organic layers were combined and washed with water (10 mL) and brine (10 mL), dried over MgSO4, filtered and evaporated to afford pure 5-tert-butyl-1-(4-chloro-3-(trifluoromethyl)phenyl)-1H-pyrazole-4-carboxylic acid (0.766 g, 83%).

1. customThe resulting mixture was evaporated
2. customto remove the methanol
3. washwashed with ether (20 mL)
4. extractionextracted with ethyl acetate (2×30 mL) The organic layers
5. washwashed with water (10 mL) and brine (10 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated