反应详情

To a suspension of 5-chloro-2-(2,3-difluoro-6-methoxybenzyloxy)anisole (8.6 g) in acetic anhydride (54 mL) was added 60% nitric acid (2.9 mL) in a dropwise manner under ice-cooling, and the mixture was stirred under ice-cooling for 30 minutes. To the reaction mixture was added water (54 mL) in a dropwise manner, and the resulting mixture was stirred under ice-cooling for 30 minutes. The precipitated crystals were collected by filtration. The collected crystals were washed with water and a mixed solvent (n-hexane/ethanol=4/1), and dried under reduced pressure to give the title compound (9.41 g).

1. temperaturecooling
2. temperaturecooling for 30 minutes
3. stirringthe resulting mixture was stirred under ice-
4. temperaturecooling for 30 minutes
5. filtrationThe precipitated crystals were collected by filtration
6. washThe collected crystals were washed with water
7. dry with materiala mixed solvent (n-hexane/ethanol=4/1), and dried under reduced pressure