反应详情

To a solution of 4-[2-(4-fluorophenyl)-2-oxoethyl]benzoic acid (0.100 g, 0.387 mmol) in acetonitrile was added proton sponge ((0.083 g) and diphenylphosphoryl azide (0.106 g). The reaction mixture was refluxed for 30 minutes. 2,5-dimethyl aniline (0.047 g, 0.388 mmol) was added and the mixture was refluxed another 30 minutes. The reaction was quenched with HCl 1 M and extracted with ethyl acetate, dried over sodium sulfate, filtered and evaporated to dryness. The residue was purified using flash chromatography eluting with hexane/ethyl acetate 40% to give (0.052 g) of the title compound.

1. temperatureThe reaction mixture was refluxed for 30 minutes
2. temperaturethe mixture was refluxed another 30 minutes
3. customThe reaction was quenched with HCl 1 M
4. extractionextracted with ethyl acetate
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customevaporated to dryness
8. customThe residue was purified
9. washeluting with hexane/ethyl acetate 40%