2,3-二氯苯基哌嗪合成方法的改进(英文)

Process development of the synthesis of 2,3-dichlorophenylpiperazine

2,3-二氯苯胺硫酸盐经重氮化,再与KI置换生成相应的芳基碘化物,产率81%。芳基碘化物与哌嗪在二甲基亚砜中反应,CuI和脯氨酸为催化剂,收率20%。该方法操作简单,对湿不敏感,产物易于分离,具有一定的实用价值。

The new pathway for the synthesis of 2, 3-dichlorophenylpiperazine from cheap raw material, 2, 3-dichloroaniline is presented. The hydrogen sulphate salt of 2, 3-dichloroaniline was converted to the corresponding Aryl Iodide in good yield of 81% by reacting with conc. H2SO4 and NaNO2 to form intermediate diazonium salt, which was further displaced by KI. The desired product was obtained by reacting Aryl Iodide and piperazine in the presence of CuI as catalyst, proline as ligand, K2CO3 as base and dimethyl sulfoxide as solvent with yield of 20 %. The method is simple, utilizes cheap catalyst and ligand, insensitive to moisture; it is easy to separate the product, and can undergo large-scale production.