反应详情

5-Amino-2-nitro-benzoic acid (compound A′) (910 mg) was dissolved in methanol (50 ml). Thionyl chloride (0.74 ml) was added dropwise to the solution on an ice bath, and a reaction was allowed to proceed under reflux with heating for 12 hr. After the completion of the reaction, the reaction solution was allowed to stand for cooling to room temperature and was then concentrated under the reduced pressure. The residue was purified by column chromatography eluted with a chloroform-methanol system to give 5-amino-2-nitro-benzoic acid methyl ester (410 mg, yield 42%).

1. temperatureunder reflux
2. temperaturewith heating for 12 hr
3. customAfter the completion of the reaction
4. concentrationwas then concentrated under the reduced pressure
5. customThe residue was purified by column chromatography
6. washeluted with a chloroform-methanol system