反应详情

温度

50 °C

Add tert-butyl 4-(4-(trifluoromethyl)-1-(2-pyrrolidin-1-ylethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate succinate (120 g, 224.48 mmol) in methanol (720 mL) to 37% aqueous hydrogen chloride (76.08 mL, 4 eq) at room temperature. Stir the solution at 50° C. Concentrate the reaction mixture. Add 500 mL water and wash with methyl tert-butyl ether (200 mL). Basify the aqueous solution with 6M aqueous sodium hydroxide at 0° C. Extract with ethyl acetate (4×200 mL). Dry the organics over anhydrous sodium sulfate and concentrate in vacuo to give the title compound (68 g, 96%). MS (ES) m/z=317 [M]+.

1. concentrationConcentrate the reaction mixture
2. additionAdd 500 mL water
3. washwash with methyl tert-butyl ether (200 mL)
4. customat 0° C
5. extractionExtract with ethyl acetate (4×200 mL)
6. dry with materialDry the organics over anhydrous sodium sulfate
7. concentrationconcentrate in vacuo