1-Nitro-2,5-bis(trifluoromethyl)benzene → 2,5-Bis(trifluoromethyl)aniline

温度

50 °C

To a solution of 2-nitro-1,4-bis(trifluoromethyl)benzene (3.3 g, 12.7 mmol) in methanol (15 mL) was added a solution of SnCl2.H2O (8.57 g, 38.1 mmol) in conc. HCl (15 mL) at room temperature, and the mixture was heated to 50° C. and stirred for 4 hours. Methanol was removed, and the aqueous solution was basified with conc. NaOH solution until pH 10. The suspension was diluted with EtOAc (100 mL), and the mixture was stirred at room temperature for 30 minutes and filtered. The solid was discarded, and the filtrate was washed with brine (50 mL), dried over sodium sulfate, and filtered. The solution was concentrated to give 2,5-bis(trifluoromethyl)benzenamine as a yellow oil (2.5 g). MS (ESI): m/z 230 [M+H]+.

1. customMethanol was removed
2. additionThe suspension was diluted with EtOAc (100 mL)
3. stirringthe mixture was stirred at room temperature for 30 minutes
4. filtrationfiltered
5. washthe filtrate was washed with brine (50 mL)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationThe solution was concentrated

ORDレコード

ord-0a858d2e28904dfdb0f31798423e5cef

出典データセット

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08969349B2