反应详情

2-Chloro-5-chlorosulfonylbenzoic acid (5.0 g.) is added to a solution of 4-piperidyl carbinol (6.9 g.) in 40 ml. of methylene chloride. The solution is refluxed for 2 hours, cooled to room temperature and stirred overnight. The solution is evaporated to dryness, the gummy residue dissolved in 1 N sodium hydroxide, and the alkaline solution extracted twice with ether. The aqueous solution is acidified with concentrated hydrochloric acid, and the precipitate recovered by filtration. Recrystallization from ethyl acetate yields crystals, m.p. 185°-187° C.

1. temperatureThe solution is refluxed for 2 hours
2. customThe solution is evaporated to dryness
3. dissolutionthe gummy residue dissolved in 1 N sodium hydroxide
4. extractionthe alkaline solution extracted twice with ether
5. filtrationthe precipitate recovered by filtration
6. customRecrystallization from ethyl acetate
7. customyields crystals, m.p. 185°-187° C.