反应详情

温度

0 °C

To a solution of 4-iodo-2-nitrobenzoic acid (2.3 g, 7.9 mmol) in DMF (30 mL) was added DBU (2.4 mL, 16 mmol) followed by iodomethane (1.5 mL, 24 mmol). The reaction mixture was allowed to stir at 0° C. for 15 min, then slowly allowed to warm to rt and to stir overnight. After 12 h, the reaction mixture was poured into 200 mL of H2O and extracted with EtOAc (2×100 mL). The organic solutions were combined, washed with H2O (2×100 mL), dried over Na2SO4, filtered and concentrated to give methyl 4-iodo-2-nitrobenzoate (2.3 g, 96%).

1. temperatureto warm to rt
2. stirringto stir overnight
3. waitAfter 12 h
4. extractionextracted with EtOAc (2×100 mL)
5. washwashed with H2O (2×100 mL)
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated