Acetic Acid → 2-Bromo-5-chloro-4-(trifluoromethyl)aniline

A mixture of reduced iron (17.7 g), acetic acid (290 ml) and water (145 ml) was stirred with heating at 60° C. for 15 min, 5-bromo-2-chloro-4-nitrobenzotrifluoride (17.7 g) dissolved in 1,4-dioxane (100 ml) was added thereto, and the mixture was stirred with heating at 60° C. for 30 min. The reaction mixture was ice-cooled, ethyl acetate (700 ml) was added and the mixture was stirred at room temperature, The reaction mixture was filtered through a celite (trademark) filter. The filtrate was washed three times with a 1N aqueous sodium hydroxide solution and then with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give 2-bromo-5-chloro-4-(trifluoromethyl)aniline (17.1 g, yield 100%).

1. additionwas added
2. stirringthe mixture was stirred
3. temperaturewith heating at 60° C. for 30 min
4. temperaturecooled
5. stirringthe mixture was stirred at room temperature
6. filtrationThe reaction mixture was filtered through a celite (trademark)
7. filtrationfilter
8. washThe filtrate was washed three times with a 1N aqueous sodium hydroxide solution
9. dry with materialwith saturated brine, and dried over anhydrous sodium sulfate
10. customThe solvent was evaporated under reduced pressure

ORDレコード

ord-43e193bc77b8493ca2c322b3fe39ca2a

出典データセット

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07994196B2