反应详情

温度

80 °C

According to the general method described in Synth. Commun. 2010, 40, 732, a mixture of 4-bromoaniline (10.0 g, 58.1 mmol) and 2,2-dimethyl-1,3-dioxan-4,6-dione (8.40 g, 58.1 mmol) was heated at 80° C. for 1 hour and cooled to room temperature to receive 3-((4-bromophenyl)amino)-3-oxopropanoic acid as a solid. A stream of nitrogen gas was passed over the solid product to remove liquid acetone formed as a by-product. To this solid was added Eaton's reagent (40 mL) and the mixture was heated at 70° C. for 12 hours and then cooled to room temperature. To the resulting mixture was added water and stirred vigorously to receive a suspension which was filtered. The solid residue was washed with water and dried in air to yield the title compound.

1. temperaturecooled to room temperature
2. customto remove liquid acetone
3. customformed as a by-product
4. temperaturethe mixture was heated at 70° C. for 12 hours
5. temperaturecooled to room temperature
6. filtrationwas filtered
7. washThe solid residue was washed with water
8. customdried in air