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 resulting mixture was stirred for 20 minutes while cooling on ice. After adding 28% aqueous ammonia to the mixture and stirring at room temperature for 2 hours, ethyl acetate was further added. After then 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 the solvent in the filtrate was distilled off under reduced pressure. The obtained residue (solid) was washed with diethyl ether and collected by filtration to obtain the title compound (11.8 g, 45.4 mmol).

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