反应详情

温度

90 °C

To a round bottom flask was added 4-bromo-2-fluoro-1-nitrobenzene (11.8 g, 53.7 mmol), anhydrous 1,4 Dioxane (100 mL), and a 2.0 M solution of methyl amine in methanol (56.4 mL, 113 mmol). The reaction mixture was then heated to 90° C. while stirring in a hot oil bath with a water cooled reflux condenser attached under an atmosphere of nitrogen for 3.5 hours. The crude reaction mixture was then allowed to cool to room temperature, and concentrated to give 5-bromo-N-methyl-2-nitroaniline (1-1). MS (M)+: observed=230.9, calculated=231.05.

1. temperaturecooled
2. temperaturereflux condenser
3. customThe crude reaction mixture
4. temperatureto cool to room temperature
5. concentrationconcentrated