Abstract: No-carrier-added meta-*Iiodobenzylguanidine((n.c.a.)^123/131IMIBG) has been considered to be promising diagnostic agents for oncology and cardiology, or as targeted radiotherapeutics for neuroendocrine tumors. The synthesis of a fluorous supported precursor for the purification without HPLC of n.c.a.*IMIBG was presented and its structure was determined. The precursor was labeled with radioactive iodine and the preliminary biodistribution of n.c.a.*IMIBG was studied. The uptake of n.c.a.¹²⁵IMIBG were significantly higher than that of c.a.¹²⁵IMIBG in heart, spleen, lung and adrenals. This facile preparation method of n.c.a.*IMIBG would allow its wider application in clinic.