A simple method of synthesis of high pure tris(8-hydroxyquinoline)aluminum (Alq3) from commercial available 5N Al2O3 and 8-hydroxyquinolinol has been developed. One-step exchange chemical reaction has been conducted under controlled 8-hydrixyquinoline vapor at a temperature of 190–240 °C with water removal by phosphorus anhydride. According to analysis of inductively coupled plasma mass-spectrometry, the chemical purity of synthesized Alq3 was 99.998 wt%. Photoluminescence of the synthesized Alq3 has been measured and slightly differed from those of Alq3 obtained by traditional organic synthesis.