反应详情

3-(2-Iodo-6-nitro-phenyl)-2-oxo-propionic acid 74c (2.086 g, 6.2 mmol) was dissolved in 6 ml of methanol under stirring, and added with 20 ml of water and 7 ml of hydrogen peroxide to the solution at room temperature. Upon completion of the addition, the reaction mixture was stirred at room temperature for 1 hour. After thin lay chromatography showed the disappearance of starting materials, the reaction mixture was filtered, extracted with ethyl acetate (20 ml×2). The combined organic extracts were concentrated under reduced pressure, combined with the above filter cake, and dried to obtain the title compound (2-iodo-6-nitro-phenyl)-acetic acid 74d (1.77 g, yield 70%) as a brown solid.

1. additionUpon completion of the addition
2. stirringthe reaction mixture was stirred at room temperature for 1 hour
3. filtrationthe reaction mixture was filtered
4. extractionextracted with ethyl acetate (20 ml×2)
5. concentrationThe combined organic extracts were concentrated under reduced pressure
6. customdried