反应详情

温度

80 °C

After dissolving 2-amino-5-iodobenzoic acid (4 mmol, 1052 mg) in DMF (10 ml) and MeOH (5 ml), NEt3 (3 eq, 1.67 ml) was added. Next, palladium acetate (0.1 eq, 90 mg) and dppp (0.1 eq, 165 mg) were added, carbon monoxide substitution was carried out, and the mixture was stirred at 80° C. for 5 hours. Upon completion of the reaction, acetic acid (2.5 ml) was added to suspend the reaction. Water (50 ml) was added, and extraction was performed with ethyl acetate (50 ml×3 times). The organic layer was washed with water (100 ml×2 times) and then dried over sodium sulfate. After concentration, a developing solvent (Hex/AcOEt=4/1→1/1) was used for purification by silica gel chromatography to obtain 2-amino-5-(methoxycarbonyl)benzoic acid. The compound was identified by LC-MS.

1. additionwas added
2. additionwas added
3. customthe reaction
4. extractionextraction
5. washThe organic layer was washed with water (100 ml×2 times)
6. dry with materialdried over sodium sulfate
7. concentrationAfter concentration
8. customa developing solvent (Hex/AcOEt=4/1→1/1) was used for purification by silica gel chromatography