反应详情

温度

60 °C

To a solution of 4-bromo-2-methoxyaniline 7.1 g (35.1 mmol) in HCl 25% m/v 20 mL, cyanamide 20.6 g (494.3 mmol) was added in portion (1.6 g every half hour). The reaction was stirred at 60° C. for 6 hours, then cooled down to room temperature, diluted with H2O (20 mL), extracted with AcOEt (10 mL). NaOH 35% (30 mL) was added to pH>>14. The aqueous phase was extracted with AcOEt (3×50 mL), dried over Na2SO4 and concentrated to afford 8.5 g (quantitative yield) of the title compound.

1. temperaturecooled down to room temperature
2. extractionextracted with AcOEt (10 mL)
3. additionNaOH 35% (30 mL) was added
4. extractionThe aqueous phase was extracted with AcOEt (3×50 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated