Tin dichloride dihydrate → 3,6-Bis(trifluoromethyl)benzene-1,2-diamine

Temperatur

50 °C

To a solution of 2-nitro-3,6-bis(trifluoromethyl)benzenamine (2.3 g, 8.4 mmol) in methanol (10 mL) was added a solution of SnCl2.H2O (7.56 g, 33.6 mmol) in concentrated HCl (15 mL). The mixture was heated to 50° C. and stirred for 2 hours. Methanol was removed in vacuum and the aqueous solution was basified with sodium hydroxide solution. The suspension was diluted with EtOAc (150 mL), and the mixture was stirred at room temperature for 30 minutes and filtered. The filtrate was washed with brine (100 mL), dried over sodium sulfate, and filtered. The solution was concentrated to give a crude product of 3,6-bis(trifluoromethyl)benzene-1,2-diamine (1.5 g). MS (ESI): m/z 245 [M+H]+

1. customMethanol was removed in vacuum
2. additionThe suspension was diluted with EtOAc (150 mL)
3. stirringthe mixture was stirred at room temperature for 30 minutes
4. filtrationfiltered
5. washThe filtrate was washed with brine (100 mL)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationThe solution was concentrated

ORD-Eintrag

ord-a1497c955a2142be9dea65c796d4b299

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08969349B2