反应详情

6.31 g (14.9 mmol) of 2-[4-[N-acetyl-N-(3-chloropropyl) amino]-3-fluorophenyl]-5-amino-6,8-difluoro-4H-1-benzopyran-4-one obtained in Example 50 was dissolved in 240 mL of methyl ethyl ketone, 6.09 g (149 mmol) of sodium iodide was added and the mixture was heated at reflux for 4 hours. The reaction solution was cooled to room temperature and filtered. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (chloroform-chloroform:methanol=50:1) to give 7.17 g of 2-[4-[N-acetyl-N-(3-iodopropyl)amino]-3-fluorophenyl]-5-amino-6,8-difluoro-4H-1-benzopyran-4-one (yield: 93%).

1. temperaturethe mixture was heated
2. temperatureat reflux for 4 hours
3. filtrationfiltered
4. distillationThe solvent was distilled off under reduced pressure
5. customthe residue was purified by silica gel column chromatography (chloroform-chloroform:methanol=50:1)