反应详情

温度

120 °C

To the mixture of 4-(4-chloro-3-(trifluoromethyl)phenoxy)benzaldehyde (600 mg, 1.996 mmol), ammonium acetate (77 mg, 0.998 mmol) in AcOH (5 mL) was added nitromethane (0.323 mL, 5.99 mmol). It was heated at 120° C. for 3 h, then concentrated in vacuo. The residue was dissolved in DCM (30 ml), washed with saturated NaHCO3 aqueous solution (20 ml×2), and brine. The organic phase was collected, dried over Na2SO4, filtered, concentrated to provide the title compound as a brown solid (680 mg, 66.4% yield), which was used without further purification. LCMS: rt=4.17 min, [M+H+]=344.1

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in DCM (30 ml)
3. washwashed with saturated NaHCO3 aqueous solution (20 ml×2), and brine
4. customThe organic phase was collected
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated