反应详情

3 g (4.08 mmol) of 2,2-bis-(3-nitro-4-tosyloxyphenyl)hexafluoropropane was dissolved in 70 ml of butyl acetate, followed by moderately heating and refluxing. Then 5.26 ml (40.8 mmol) of n-methylbenzylamine was added dropwise into the solution, and after heating and refluxing were continued for 12 hours, the solution was cooled to room temperature. After 20 ml of dilute hydrochloric acid was added and extraction with ethyl acetate was carried out two times, an organic layer was washed with dilute hydrochloric acid, an aqueous solution of sodium hydrogencarbonate and saturated brine. After the washed organic layer was dried with anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The obtained liquid product was separated by silica gel chromatography (hexane/ethyl acetate=4/1, hexane/dichloromethane=1/1) to obtain 2.1 g (yield: 81%) of 2,2-bis-[3-nitro-4(N-methyl-N-benzylamino)phenyl]hexafluoropropane in the form of yellow solid.

1. temperatureby moderately heating
2. temperaturerefluxing
3. temperatureafter heating
4. temperaturerefluxing
5. extractionextraction with ethyl acetate
6. washan organic layer was washed with dilute hydrochloric acid
7. dry with materialAfter the washed organic layer was dried with anhydrous magnesium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. customThe obtained liquid product was separated by silica gel chromatography (hexane/ethyl acetate=4/1, hexane/dichloromethane=1/1)