摘要
以对氨基苯磺酰胺、双氧水和盐酸为原料合成3,5二氯对氨基苯磺胺,研究了原料配比、催化剂AlCl3的滴加方式、H2O2的滴加时间对收率的影响,得出最佳工艺条件为:n(C6H6N2O2S)∶n(30%HCl质量分数)=1∶13.7,7gAlCl3晶体溶于剩余的盐酸中,于H2O2滴加一半时加入,H2O2的滴加时间为40min。产品的收率可达81.0%,熔点为204~205.5℃。
3,5-dichlorosulfanilamide was synthesized from sulfanilamide,hydrogen peroxide and hydrochloric acid. The effect of mixture ratio, the addition form of AlCl_3, the addition time of H_2O_2 on yield of 3,5-dichlorosulfanilamide were investigated.The optimum conditions for synthesis are as follows:the mole ratio of C_6H_6N_2O_2S to 30%HCl is 1∶13.7, 7 g AlCl_3 is dissolved in residual hydrochloric acid and added in half amount of H_2O_2, the addition time of H_2O_2 is 40 min.The yield of product is 81.0%, melting point is 204~205.5℃.
出处
《应用化工》
CAS
CSCD
2005年第2期115-116,共2页
Applied Chemical Industry