反应详情

温度

50 °C

Add 5 M hydrogen chloride in isopropyl alcohol (112.7 mL, 5.0 eq) to a solution of tert-butyl 4-(1-(2-(pyrrolidin-1-yl)ethyl)-4-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-2-yl)piperidine-1-carboxylate (132.0 g, 274.61 mmol) in isopropyl alcohol (549 mL). Stir the reaction mixture at 50° C. for six hours. Concentrate in vacuo. Dilute with water (1 L) and adjust the pH to 12 with 2 M aqueous sodium hydroxide. Extract with ethyl acetate and dichloromethane. Dry the organics over anhydrous magnesium sulfate and concentrate in vacuo to give 4-(1-(2-pyrrolidin-1-yl-ethyl)-4-(tetrahydro-pyran-4-yl)-1H-imidazol-2-yl)-piperidine (81.9 g, 90%). MS (ES) m/z=333 [M]+.

1. concentrationConcentrate in vacuo
2. additionDilute with water (1 L)
3. extractionExtract with ethyl acetate and dichloromethane
4. dry with materialDry the organics over anhydrous magnesium sulfate
5. concentrationconcentrate in vacuo