4,4’-dihydroxy-3,3’-dinitrobenzophenone was synthesized by chloroben- zene and chlorobenzoyl chloride through three-step reactions, which were Friedel- Crafts acylation reaction, nitration reaction by mixed acid, and alkaline hydrolysis reaction in alcohol-water medium. The total yield of 4,4’-dihydroxy-3,3’-dinitrobenz- ophenone was 78.34%. Analysis such as FT-IR, MS, 1HNMR and HPLC were used to analyze the structure and purity of products. Single factor experiment was used to study on the process of alkaline hydrolysis reaction and got the optimism condition, under which the yield of the crude product was 96.71%, and its purity was 97.11%. In order to obtain purer product, using DMF and ethanol to recrystallize the crude product can improve the purity of product to 99.30%, and the reycrystallization yield was 81%.