反应详情

To a suspension of 5-bromo-2-trifluoromethoxy-phenylamine (5.0 g, 19.5 mmol) in EtOH (15 mL), cyanamide (1.64 g, 39 mmol) dissolved in 5 mL of EtOH and 1 mL H2O, and HCl 37% (3.25 mL) diluted in 10 mL EtOH were added drop wise into the mixture under stirring. The mixture was refluxed for 72 h. The mixture was cooled down to room temperature, concentrated then diluted with water; NaOH 1N was added to basic pH and extracted several times with ethyl acetate, dried over sodium sulfate and concentrated to afford 5.2 g of the title compound (89% yield).

1. additionwere added drop wise into the mixture
2. temperatureThe mixture was refluxed for 72 h
3. concentrationconcentrated
4. additionthen diluted with water
5. additionNaOH 1N was added to basic pH
6. extractionextracted several times with ethyl acetate
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated