摘要
以3-甲基苯胺为原料,磺酸占位,以盐酸和双氧水作为氯化试剂氯化,脱磺酸基得到2,4,6-三氯-3-甲基苯胺,纯度达到99%以上;以3-甲基苯胺为原料,用乙酸酐进行氨基保护,磺酰胺基占位,去乙酰基,用盐酸和双氧水氯化,最后水解得到2,6-二氯-3-甲基苯胺,纯度达到99.4%以上,总收率50%左右。所得产品通过熔点测定,核磁、红外谱图进行表征。
2,4,6-Trichloro-3-methylaniline was prepared with 3-methylaniline as the starting material, which was first treated with sulfonic acid, followed by chlorinated with hydrochloric acid and aquae hydrogenii dioxide. Then the chlorinated compound was hydrolyzed to get the final product, with purity more than 99%. 2,6-Dichloro-3-methylaniline was prepared with 3-methylaniline as the staring material, which was first N-acetylated with acetic anhydride, then treated with chlorosulphonic acid and ammonia yielding the intermediate（2-methyl-4-（N-acetyl）-benzenesulfonic amide）, which was followed by deacetylateing, chlorinated and hydrolyzed to get the final product, with purity more than 99.4% and yield of the product attained 50%. The synthesized products were characterized by NMR and IR.
出处
《农药》
CAS
北大核心
2008年第4期261-262,266,共3页
Agrochemicals
