反应详情

温度

0 °C

To a stirred solution of (3-(8-(1,3-dioxolan-2-yl)octyloxy)phenyl)-(phenyl)-methanamine (0.62 g, 1.62 mmol) in pyridine (10 mL) at 0° C., (R)-quinuclidin-3-yl carbonochloridate (0.48 g, 2.1 mmol) was added. The reaction was stirred at 0° C. for 1 hour and then allowed to warm to RT for 16 hours. Water was added to the reaction mixture and extracted with ethyl acetate (×3). The combined extracts were washed with brine, dried (sodium sulfate), filtered, and concentrated under reduced pressure. The crude material was purified by chromatography on a KP-NH Biotage cartridge eluting with 0-20% methanol in ethyl acetate to afford the title compound (0.67 g, 78%).

1. temperatureto warm to RT for 16 hours
2. extractionextracted with ethyl acetate (×3)
3. washThe combined extracts were washed with brine
4. dry with materialdried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified by chromatography on a KP-NH Biotage cartridge
8. washeluting with 0-20% methanol in ethyl acetate