反应详情

tert-Butyl 3-(2-(perfluorophenoxysulfonyl)ethyl)piperidine-1-carboxylate (0.5 g, 1.09 mmol) and 4-(2-pyrrolidinoethyl)piperidine (0.4 g, 2.18 mmol) were dissolved in tetrahydrofuran (10 ml), 1,8-diazabicyclo[5.4.0]undec-7-ene (0.5 ml, 3.27 mmol) was added under an inert gas and the mixture was refluxed for 2 h. Ethyl acetate and saturated sodium bicarbonate solution (20 ml of each) were added, the phases were separated and the aqueous phase was extracted with ethyl acetate (2×30 ml). The combined organic phases were washed with saturated sodium chloride solution (20 ml), dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with ethyl acetate/methanol/ammonia (25% aq) (300:100:1). Yield: 0.32 g (64%)

1. temperaturethe mixture was refluxed for 2 h
2. customthe phases were separated
3. extractionthe aqueous phase was extracted with ethyl acetate (2×30 ml)
4. washThe combined organic phases were washed with saturated sodium chloride solution (20 ml)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by column chromatography (silica gel) with ethyl acetate/methanol/ammonia (25% aq) (300:100:1)