反应详情

To a solution of 2-iodobenzoic acid (6.4 g, 25.8 mmol) in THF (90 mL) is added HOBt (3.5 g, 25.8 mmol). After the mixture is stirred at RT for 10 min, EDCl (4.93 g, 25.8 mmol) is added followed by triethylamine (4.9 mL, 34.4 mmol). The mixture is stirred at RT for 40 min then amino-(2-iodophenyl)-acetic acid methyl ester (5.0 g, 17.2 mmol) is added and stirring is continued for 18 h. The solvent is removed under reduced pressure and water is added to the residue. The mixture is extracted with EtOAc and the organic phase is washed with brine and dried over magnesium sulfate. The solvent is removed under reduced pressure and the residue purified by flash chromatography using a gradient of 0-60% EtOAc/hexane as eluent to give the title compound.

1. stirringThe mixture is stirred at RT for 40 min
2. stirringstirring
3. waitis continued for 18 h
4. customThe solvent is removed under reduced pressure and water
5. additionis added to the residue
6. extractionThe mixture is extracted with EtOAc
7. washthe organic phase is washed with brine
8. dry with materialdried over magnesium sulfate
9. customThe solvent is removed under reduced pressure
10. customthe residue purified by flash chromatography