四取代全氟辛基金属酞菁的合成

Synthetic of Tetra-substituted Perfluorooctane Metal Phthalocyanine

以邻苯二甲酰亚胺为起始原料,在30%的发烟硫酸条件下经碘化得到3-碘邻苯二甲酰亚胺,氨解、脱水得到3-碘邻苯二甲腈,并与全氟辛基碘在铜粉催化作用下,生成3-全氟辛基邻苯二甲腈,选用DBU合成法得到了标题化合物。对3-碘邻苯二甲酰亚胺的合成条件进行考察,得到了最佳反应条件:反应温度为60℃,n(邻苯二甲酰亚胺)∶n(单质碘)=1∶1,反应时间为12 h。目标产物结构经1HNMR和HRMS确认。

In order to synthesize a new precursor of phthalocyanine compounds,3-iodo-phthalimide was obtained by iodization of phthalimide in 30% fuming sulfuric acid catalytic conditions. After ammonolysis,dehydration,3-iodophthalonitrile was obtained.3-Perfluorooctane phthalonitrile was synthesized by using 3-iodophthalo-nitrile,copper,perfluorooctyl iodide. The DBU method of synthetic phthalocyanine was choosed. The effect of synthesis of 3-iodo-phthalimide reaction conditions was investigated to determine the optimum reaction conditions as follows. The reaction temperature was 60 ℃,n（ phthalimide） ∶ n（ iodine） = 1∶ 1,the reaction time was 12 h. The structures of the intermediates and target product were confirmed by1 HNMR and HRMS.