金属卟啉类化合物的合成

Synthesis of Metalloporphyrins

研究了溶剂,金属盐试剂,反应温度,反应时间等因素对金属卟啉化合物合成的影响,合成并表征了铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)、锌(Ⅱ)的次卟啉(Ⅸ)二甲酯及3-(乙酰基)次卟啉(Ⅸ)二甲酯的金属化合物。结果表明,采用DMF单一溶剂可大幅提高镍(Ⅱ)和锌(Ⅱ)次卟啉(Ⅸ)二甲酯的产率至98%左右,而且反应时间由二氯甲烷/甲醇体系的2h减至0.5h,溶剂用量由150mL降为20mL。后续提纯不必采用萃取法,而只需减压回收溶剂,然后水洗除去无机盐即可。

Traditionally the synthesis of metallodeuteroporphyrins-Ⅸ-dimethylester is carried out in a system of CH2Cl2/CH3OH, but the yields of nickel（ Ⅱ ） and zinc（ Ⅱ） deuteroporphyrins in the system are very low, both less than 50%. In this paper, the effects of solvent, metal-salt, reaction temperature and reaction time on the synthesis of metal-porphyrins were investigated. Cu（ Ⅱ ）, Co（ Ⅱ ）,, Ni（ Ⅱ） and Zn（ Ⅱ ） metallodeu- teroporphyrin-Ⅸ-dimethylesters and their metal-3-acetyldeuteroporphyrin-Ⅸ-dimethylesters were synthesized and characterized. The yields of Ni （ Ⅱ ） and Zn （ Ⅱ ） metallodeuteroporphyrin-Ⅸ-dimethylesters were increased greatly to about 98% when DMF was used as the solvent; at the same time, the reaction time decreased from 2 h in the CH2Cl2/CH3OH system to 0. 5 h and the amount of solvent decreased from 150 mL to 20 mL. And the purification of products was carried out simply by reclaiming solvent under reduced pressure first and then removing inorganic salts by washing the residue with water instead of by extraction method which consumes large amount of solvent.