反应详情

温度

95 °C

To a mixture of 3,3-dimethyl-2-(3-nitro-phenyl)-6-trifluoromethyl-1,2,3,4-tetrahydro-quinoline (2.4 g, 6.8 mmol) in ethanol 95% (100 mL) and 10% hydrochloric acid (5 mL) was added iron (1.2 g, 20 mmol). The reaction mixture was stirred at 95° C. for 3 h. Then the insoluble solid was filtered off and the filtrate was concentrated in vacuo and the residue was extracted with ethyl acetate (2×200 mL), washed with 30% sodium hydroxide in water (2×100 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to afford 3-(3,3-dimethyl-6-trifluoromethyl-1,2,3,4-tetrahydro-quinolin-2-yl)-phenylamine (1.8 g, 86%) as a brown solid: LC/MS m/e calcd for C18H19F3N2 (M+H)+: 321.36, observed: 321.1.

1. filtrationThen the insoluble solid was filtered off
2. concentrationthe filtrate was concentrated in vacuo
3. extractionthe residue was extracted with ethyl acetate (2×200 mL)
4. washwashed with 30% sodium hydroxide in water (2×100 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo