一种改进的制备间硝基苯乙酮方法

An Improved Way to Prepare m-Nitroacetophenone

以KNO3和磷酸构成的复合硝化剂对0.1 moL苯乙酮进行硝化,元素分析、FTIR和1HNMR的分析结果表明,硝化得到的产物为间硝基苯乙酮。研究表明,苯乙酮以KNO3-磷酸复合硝化剂硝化时,反应具有性能缓和、安全性高、可控性强的特点,反应温度可由混酸硝化时的-15^-10℃提高至80~90℃,且氧化副反应的发生程度显著降低,苯乙酮的可利用率提高。在n(硝酸钾)/n(苯乙酮)为1.5~1.7、n(磷酸)/n(硝酸钾)为1.6~2.0、反应温度为80~90℃、反应时间为7.0~8.0 h时,间硝基苯乙酮收率可达45%左右。

A nitration mixture consisting of KNO3 and phosphoric acid was used to nitrify 0. 1 mol acetophenone. Elementary analysis, FTIR and 1HNMR indicated that the product was mnitroacetophenone. Experimental results showed that, with KNO3-phosphoric acid as nitrifying agent, the nitration reaction of acetophenone was mild, safe and easy to control. Compared with the nitration reaction using common mixed acid, the reaction temperature could be raised to 80. 0～90.0℃ from -15～- 10℃, the side reaction of oxidation could be reduced and the utilization ratio of acetophenone could be increased obviously. When n （ KNO3 ）/n （ acetophenone ） was 1.5 to 1.7, n （ H3 PO4 ）/n （ KNO3 ） was 1.6 to 2. 0, reaction temperature was 80. 0 to 90. 0 ℃, and reaction time was 7.0 to 8.0 h, the yield of m-nitroacetophenone could be up to 45 %.