反应详情

温度

50 °C

Combine tert-butyl 4-(1-(2-(methylsulfonyloxy)ethyl)-4-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-2-yl)piperidine-1-carboxylate (2.02 g, 4.42 mmol), pyrrolidine (1.1 mL, 3.0 eq), and dimethylformamide (19 mL). Heat the reaction mixture to 50° C. overnight. Dilute with dichloromethane and saturated aqueous sodium bicarbonate. Separate the layers. Wash the organics with water. Dry the organics over anhydrous sodium sulfate, filter, and concentrate in vacuo. Purify by silica gel chromatography, eluting with hexanes to ethyl acetate to 10% methanol in dichloromethane, to give the title compound as a yellow oil (1.79 g, 93%). MS (ES) m/z=433 [M]+.

1. customSeparate the layers
2. washWash the organics with water
3. dry with materialDry the organics over anhydrous sodium sulfate
4. filtrationfilter
5. concentrationconcentrate in vacuo
6. customPurify by silica gel chromatography
7. washeluting with hexanes to ethyl acetate to 10% methanol in dichloromethane