反应详情

温度

50 °C

To a solution of 2-amino-3-nitrobenzoic acid (prepared using the procedure as described in U.S. Pat. No. 6,737,421, EXAMPLE 2, part b) in dimethoxyethane (DME, 7.1 mL/g), was added thionyl chloride (1.33 equivalents). The mixture was stirred at 50° C. for 12 hours, cooled and slowly added to concentrated ammonium hydroxide (22 equivalents). The mixture was stirred at 50° C. for 2 hours, water was added, and the mixture was cooled and filtered. The solid was washed with water and isopropanol, and dried under vacuum to give the title compound (89% yield).

1. temperaturecooled
2. stirringThe mixture was stirred at 50° C. for 2 hours
3. temperaturethe mixture was cooled
4. filtrationfiltered
5. washThe solid was washed with water and isopropanol
6. customdried under vacuum