反应详情

温度

40 °C

To a mixture of 4-Bromo-3,5-diethoxybenzoic acid (2.8 g) in DMF (25 ml) was added CDI (1.8 g) at room temperature and the mixture was stirred at 40° C. for 2 h. To the reaction mixture, t-BuOH (1.85 ml) and DBU (1.75 ml) were added and further stirred at 40° C. overnight. After cooling to room temperature, the mixture was poured into ice-H2O and extracted with EtOAc. The organic layer was washed with H2O, brine and dried over sodium sulfate. After filtration and concentration, the residue was purified by silica gel column chromatography (hexane/EtOAc) to give the intended compound as a colorless solid.

1. stirringfurther stirred at 40° C. overnight
2. temperatureAfter cooling to room temperature
3. extractionextracted with EtOAc
4. washThe organic layer was washed with H2O, brine
5. dry with materialdried over sodium sulfate
6. filtrationAfter filtration and concentration
7. customthe residue was purified by silica gel column chromatography (hexane/EtOAc)