Abstract: 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) metallodeuteroporphyrin-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.