Zinc oxyacetate (Zn4O(OAc)(6)) can be prepared using a facile and green method, in which Zn(OAc)(2) and the green chemical dimethyl carbonate are used as raw materials. During Zn4O(OAc)(6) formation, the hydrolysis of dimethyl carbonate produces methanol. Zn(OAc)(2) reacts with the in situ generated methanol to form Zn4O(OAc)(6). When the H2O content is less than or equal to 0.086 wt%, Zn4O(OAc)(6) can be successfully prepared. A high Zn4O(OAc)(6) yield (>90%) can be achieved when the H2O content is between 0.053 and 0.086 wt%.