反应详情

温度

100 °C

To a solution of 5-bromo-N1-methylbenzene-1,2-diamine (7.4 g, 37 mmol) in trimethyl orthoformate (100 mL) was added p-toluenesulfonic acid (0.36 g, 1.9 mmol). The reaction mixture was heated at 100° C. for 4 h, cooled, concentrated, dissolved in ethyl acetate, washed with brine, dried over sodium sulfate and concentrated. The crude product was used in next step without further purification. (7.3 g, yield 93%) MS (ESI+) e/z: 212.1.

1. temperaturecooled
2. concentrationconcentrated
3. dissolutiondissolved in ethyl acetate
4. washwashed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe crude product was used in next step without further purification