4,4'-二羟基-3,3'-二硝基二苯甲酮的合成

Preparation of 4,4’- Dihydroxy -3,3’-dinitrobenzophenone

摘要:

以氯苯和对氯苯甲酰氯为原料，经傅克酰基化、混酸硝化、混合溶剂碱性水解3步反应制备4,4’-二羟基-3,3’-二硝基二苯甲酮，总收率78.34%。通过红外光谱、质谱、氢谱以及高效液相色谱对产品进行表征。采用单因素实验法对水解反应工艺进行考察，确定了最佳工艺条件。在该条件下粗水解产物收率为96.71%，纯度为97.11%。用DMF和异丙醇对水解产物进行重结晶，重结晶后产品收率为81%，纯度为99.30%。

Abstract:

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%.