反应详情

A mixture of 19.3 g (0.07 mole) of α,α -diphenyl-4-piperidinemethanol, 17.1 g (0.08 mole) of 5-chloro-4'-fluorovalerophenone, 20.0 g (0.2 mole) of potassium bicarbonate, and 0.1 g of potassium iodide in 250 ml of toluene and 35 ml of water is stirred on a steam bath for 70 hours. The organic layer is separated and combined with two 50 ml toluene extracts of the aqueous layer. The combined organic material is washed with water and saturated sodium chloride solution, dried over magnesium sulfate and filtered. The filtrate is diluted with about 200 ml of ether then made acidic with ethereal HCl. The resulting precipitate is recrystallized from methanol-butanone to give 4'-fluoro-5-[4-(α-hydroxy-α-phenylbenzyl)piperidino]valerophenone hydrochloride, M.P. 177°-179°C.

1. customThe organic layer is separated
2. washThe combined organic material is washed with water and saturated sodium chloride solution
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. additionThe filtrate is diluted with about 200 ml of ether
6. customThe resulting precipitate is recrystallized from methanol-butanone