间二硝基苯偶酰的合成新工艺

New technique on synthesis of m-dinitrobenzil

以苯甲醛为原料,经过自身缩合、氧化、硝化合成间二硝基苯偶酰。重点考察了硝化反应工艺条件对影响反应的因素,对反应温度、混酸浓度、反应时间等进行了优选,硝化反应的最佳条件为:苯偶酰3 g(14mmol),浓硝酸4 mL,VH2SO4∶VNHO3∶VH2O=9∶4∶4,反应温度140℃,反应时间3 h,产品收率达86.4%。目标产物的结构利用IR、MS和1H NMR进行表征。

M-dinitrobenzil was synthesized from the raw material of benzald through self-condention, oxidation, nitration. The nitration process conditions were studied on emphasis, and factors of affecting reaction such as reaction temperature, concentration of mixed acid and reaction time were optimized. The best conditions of nitration reaciton is：3 g benzil （14 mmol）,4 mL concentrated nitric acid, VH2SO4 ： VHNO3 ： VH2O = 9：4 ： 4,140 ℃ reaction temperature, 3 h reaction time and 86.4 % yield of product. The structure of goal products were confirmed by IR, MS, ^1H NMR.