论文部分内容阅读
以氯乙酰氯、对碘苯胺为原料,经酰化合成了4-碘-氯乙酰苯胺;接着分别与吡啶、1-甲基咪唑反应得到N-(4-碘苯氨基甲酰甲基)吡啶氯盐和3-甲基-1-(4-碘苯氨基甲酰甲基)咪唑氯盐;随后分别在水溶液中发生阴离子交换,合成了相应的四氟硼酸盐;对应的四氟硼酸盐在新制过氧乙酸中氧化得到两种新的离子负载的新型二(乙酰氧基)碘苯试剂{N-[(4-二乙酰氧基碘)苯氨基甲酰甲基]吡啶四氟硼酸盐}和{3-甲基-1-[(4-二乙酰氧基碘)苯氨基甲酰甲基]咪唑四氟硼酸盐}。以吡啶离子负载试剂的合成为例,对反应条件进行了探讨。化学结构用IR、1HNMR、13CNMR、MS、元素分析表征。
Chloroacetyl chloride and p-iodoaniline were used as starting materials to synthesize 4-iodo-chloroacetanilide by acylation. Then the corresponding compounds were reacted with pyridine and 1-methylimidazole to obtain N- (4-iodophenylcarbamoylmethyl) pyridine Chloride and 3-methyl-1- (4-iodophenylcarbamoylmethyl) imidazolium chloride salt, respectively; followed by anion exchange in aqueous solution to synthesize the corresponding tetrafluoroborate; the corresponding tetrafluoroboric acid Oxidation of salts in freshly prepared peracetic acid gave two new ionic supported novel bis (acetoxy) iodobenzene reagents {N - [(4-diacetoxyiodo) phenylcarbamoylmethyl] pyridine tetrafluoroborate Acid salt} and {3-methyl-1- [(4-diacetoxyiodo) phenylcarbamoylmethyl] imidazole tetrafluoroborate}. Taking the synthesis of pyridinium ion loading reagents as an example, the reaction conditions were discussed. The chemical structure was characterized by IR, 1HNMR, 13CNMR, MS, elemental analysis.