反应详情

To a mixture of 4-bromo-3,5-dimethoxybenzoic acid (15 g, 57.6 mmol) and THF (200 mL), were added triethylamine (9.63 mL, 69.0 mmol) and ethyl chloroformate (5.79 mL, 60.6 mmol) while stirring on ice, and the mixture was stirred on ice for 20 minutes. To the mixture, 28% aqueous ammonia was added and stirred at room temperature for two hours, followed by addition of ethyl acetate. After thoroughly shaking the mixture, the organic layer was separated, and the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The mixture was filtered, and then the solvent in the filtrate was distilled off under reduced pressure. The obtained residue (solid) was washed with diethyl ether, collected by filtration to obtain the title compound (11.8 g, 45.4 mmol).

1. stirringthe mixture was stirred on ice for 20 minutes
2. stirringstirred at room temperature for two hours
3. stirringAfter thoroughly shaking the mixture
4. customthe organic layer was separated
5. washthe organic layer was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationThe mixture was filtered
8. distillationthe solvent in the filtrate was distilled off under reduced pressure
9. washThe obtained residue (solid) was washed with diethyl ether
10. filtrationcollected by filtration