反应详情

A suspension of 223 g of N-methyl-4-ethynyl-4-(4-fluoro-2-nitrophenoxy)piperidine, 2 l of dry benzene, 165 g of anhydrous potassium carbonate and 130.3 g of ethyl chloroformate was stirred at reflux for 18 hr under nitrogen. The mixture was filtered and the solvent evaporated. The residue was dissolved in ether, washed with hydrochloric acid, saturated sodium bicarbonate solution, water and saturated sodium chloride solution. The ether solution was dried over anhydrous sodium sulfate and filtered. Evaporation of solvent provided an oil, which was dried at 50°-55° (1 mm). The oil crystallized to provide 226 g (83.8%) of product, mp 56°-68°.

1. temperatureat reflux for 18 hr under nitrogen
2. filtrationThe mixture was filtered
3. customthe solvent evaporated
4. dissolutionThe residue was dissolved in ether
5. washwashed with hydrochloric acid, saturated sodium bicarbonate solution, water and saturated sodium chloride solution
6. dry with materialThe ether solution was dried over anhydrous sodium sulfate
7. filtrationfiltered
8. customEvaporation of solvent
9. customprovided an oil, which
10. customwas dried at 50°-55° (1 mm)
11. customThe oil crystallized