2-Nitrophenol-4-sulfonylamide was synthesized by sulfochlorination, ammoniation, hydrolysis from o - nitrochlorobenzene being as raw materials. The reaction conditions were optimized in material proportion, reaction temperature, reaction time. The optimum technological conditions were obtained as the follows: The molar ratio of n(o - C6ClH4NO2):n(HSO3Cl)=1:4; The raw material has been fed in batches and the ration Na2SO4 is added, reaction temperature is 140 °C, reaction time is 6 [similar to] 7 h. The product n(2-nitrochlorobenzene-4-sulfochlorides):n (NH3)=1:1.5 has been treated with ammonia water at reaction temperature 38 [similar to] 40 °C for 2 h, and treated with 30% NaOH solution at 105 °C for 3 [similar to] 4 h, and then phase transfer catalyst is added, finally after acidifying, the product can be obtained. The excellent yield was 70%. The three products obtained in above three phases were characterized by IR.