四苯基卟啉的催化合成和微波合成研究

采用溶剂催化法和微波激励法合成ｍｅｓｏ－四苯基卟啉（ＴＰＰ）．发现所用溶剂的沸点和极性、催化剂的酸度（Ｐｋａ）及反应体系中的水分含量是决定反应的主要因素．采用甲苯或二甲苯做溶剂，对硝基苯甲酸做催化剂，采用溶剂蒸除—填加同步法合成的四苯基卟啉产率达到５８．４％．同样体系采用微波激励法，３０ｍｉｎ产率达到４２％，反应速度提高了２．２倍．根据ＴＰＰ与其主要副产物四苯基二氢卟啉（ＴＰＣ）的紫外光谱特点以及分光光度法的加合性，采用双波长紫外光谱法测算产品纯度，测得重结晶纯化后产品纯度为９７．７，柱色谱纯化后产品纯度达到９９．７６％．

SYNTHESIS OF MESO-TETHAPHENYLPORPHYRINS (TPP) BY CATALYST IN SOLVENTS AND UNDER MICROWAVE IRRADATION

The synthetic methods of mesoPorphyrin(TPP) by solventcatalystreaction and under microwave irradation are explored in this paper. It was discoved that the boiling point and polarity of the solvents, acidity of the catalysts, and the content of water in the reaction system were the key factos. With pnitrobentoic acid as the catalyst in toluene or xylene and with a special solvent treatment of distilationaddition at same step, TPP was given by direct condensation of pyrrole and benzaldehyde to 58^4% of the yield. Comparing with that, 42% of the yield of TPP was got under microwave irradation by the same reaction system in 30min, faster 4^2 times that of reaction rate of the catalyst method. UV spectrum and cocomponentcalculation were used for valuing the product according to the great difference between the maximum adsorption in the UV spectrum of TPP and its main byproduct 2Hporphyrin(TPC). The purity of the product for TPP was 97^7% and 99^76% for recrystallization and column purilation respec