Nitric Acid → 4-Fluoro-3-nitro-2-methoxybenzoic acid

To 4-fluoro-2-methoxybenzoic acid (0.96 g) was added concentrated sulfuric acid (6 mL) under ice-cooling, and the mixture was stirred for 15 minutes. To the mixture was added concentrated nitric acid (0.6 mL) under ice-cooling, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture was added ice, and the resulting mixture was stirred at room temperature for 10 minutes. The mixture was extracted with ethyl acetate. The extract was washed with water twice and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. To the residue was added a mixed solvent (n-hexane/ethyl acetate=2/1), and the insoluble material was collected by filtration, and dried under reduced pressure to give the title compound (0.78 g).

1. temperaturecooling
2. temperaturecooling
3. stirringthe mixture was stirred at the same temperature for 1 hour
4. additionTo the reaction mixture was added ice
5. stirringthe resulting mixture was stirred at room temperature for 10 minutes
6. extractionThe mixture was extracted with ethyl acetate
7. washThe extract was washed with water twice
8. dry with materialbrine, and dried over anhydrous magnesium sulfate
9. customThe solvent was removed under reduced pressure
10. additionTo the residue was added a mixed solvent (n-hexane/ethyl acetate=2/1)
11. filtrationthe insoluble material was collected by filtration
12. customdried under reduced pressure

ORDレコード

ord-520ee4d53083427b9c3bfb6627d11da9

出典データセット

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09040693B2