反应详情

温度

80 °C

To a stirring mixture of 9.0 g of potassium carbonate in 100 ml of dimethylformamide was added 8.0 g of 4-(2,3,4,5,6-pentafluorophenoxy)piperidine and 9.5 g of dimethylphosphinylmethyl chloride. After stirring at 80° C. for 30 hours, the reaction mixture was cooled, poured into water, and extracted with ethyl acetate. The organic layer was washed with water followed by a saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, evaporation afforded a residue which was purified by means of high pressure liquid chromatography (silica gel; elution with 5% methanol/dichloromethane). The desired fractions were evaporated to yield a solid which was sublimed to afford 2.37 g (22.1%) of 1-[(dimethylphosphinyl)methyl]-4-(2,3,4,5,6-pentafluorophenoxy) piperidine, m.p. 120°-123° C.

1. temperaturethe reaction mixture was cooled
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationAfter filtering
6. customevaporation
7. customafforded a residue which
8. customwas purified by means of high pressure liquid chromatography (silica gel; elution with 5% methanol/dichloromethane)
9. customThe desired fractions were evaporated
10. customto yield a solid which