反应详情

Aluminium trichloride (2.6 g, 19 mmol) was added in portions to a suspension of 4-chloro-7-methoxycinnoline (0.9 g, 3.8 mmol), (J. Chem. Soc. 1955, 2100), in benzene (15 ml) and the mixture was heated at reflux for 1 hour. The solvent was removed by evaporation and the residue was partitioned between ice/water and ethyl acetate. Aqueous saturated sodium chloride solution was added and the organic layer was separated. The organic layer was washed with brine, dried (MgSO4) and the solvent removed by evaporation. The residue was triturated with ether, collected, filtered and dried under vacuum to give 4-chloro-7-hydroxycinnoline (368 mg, 53%).

1. temperaturethe mixture was heated
2. temperatureat reflux for 1 hour
3. customThe solvent was removed by evaporation
4. customthe residue was partitioned between ice/water and ethyl acetate
5. additionAqueous saturated sodium chloride solution was added
6. customthe organic layer was separated
7. washThe organic layer was washed with brine
8. dry with materialdried (MgSO4)
9. customthe solvent removed by evaporation
10. customThe residue was triturated with ether
11. customcollected
12. filtrationfiltered
13. customdried under vacuum