反应详情

温度

80 °C

4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester 6b (0.32 g, 1.09 mmol) and formamidine acetate (72 mg, 1.64 mmol) in EtOH (36 mL) are heated, with stirring, to 80° C. After 44 hours, the reaction mixture is cooled to room temperature and diluted with EtOAc and washed with water (3×), saturated NaHCO3, and brine. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure to give 0.33 g (99%) clean desired product as a solid. MS APCI (+) m/z 302.3 (M+1) detected.

1. temperaturethe reaction mixture is cooled to room temperature
2. washwashed with water (3×), saturated NaHCO3, and brine
3. dry with materialThe combined organic extracts are dried (Na2SO4)
4. concentrationconcentrated under reduced pressure