反应详情

1-Thiophen-2-yl-cycloheptanecarboxylic acid ethyl ester (Example 5c) (2.5 g) and (R) -quinuclidin-3-ol (2.08 g) were dissolved in toluene (350 mL) and sodium hydride (0.1 g) added under nitrogen. The mixture was heated to reflux for 20 hours after which the toluene was carefully distilled off to leave ˜100 mL which was cooled and washed with water (100 mL), dried (MgSO4) and evaporated. The crude product was purified by column chromatography on silica eluting with ethyl acetate/triethylamine (99/1) to afford the sub-titled compound (2.84 g).

1. temperatureThe mixture was heated
2. distillationwas carefully distilled off
3. customto leave ˜100 mL which
4. temperaturewas cooled
5. washwashed with water (100 mL)
6. dry with materialdried (MgSO4)
7. customevaporated
8. customThe crude product was purified by column chromatography on silica eluting with ethyl acetate/triethylamine (99/1)