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A novel method used to synthesize diacetone diperoxide (DADP) from acetone and hydrogen peroxide without the presence of a catalytic agent is presented. Previously reported syntheses used toluenesulfonic and m‐sulfonic acid as catalyst. DADP was prepared with a purity of 99.99 %. The melting point range (128.5–134.5 °C) is consistent with reported values. The success of the reported procedure depends...