反应详情

温度

90 °C

To methyl 4-((1-(4-((3,3-dimethyl-2-oxobutyl)carbamoyl)-2-methylphenyl)-4,4,4-trifluorobutyl)amino)benzoate (200 mg) was added phosphoryl chloride (0.5 ml) at room temperature. The reaction mixture was heated at 90° C. for 1 hr, and water was added at room temperature. The filtrate was extracted with ethyl acetate, and the extract was washed with 1M aqueous sodium hydroxide solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (155.4 mg).

1. extractionThe filtrate was extracted with ethyl acetate
2. washthe extract was washed with 1M aqueous sodium hydroxide solution and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was evaporated
5. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)