NaBH_4-I_2还原法制备N,N'-二甲基间苯二胺

Synthesis of N,N′-Dimethyl-1,3-benzenediamine by Reduction Method with NaBH_4 and I_2

以间苯二胺为原料,与酰化剂甲酸反应制得中间体N,N'-二甲酰基间苯二胺,再以NABH4-I2为还原剂合成得到产品N,N'-二甲基间苯二胺,对合成工艺进行了优化,并分析了还原机理,化合物的结构经IR,1 H NMR和MS分析确定.该法原料易得,反应条件要求低,收率高且成本更低.

The common aromatic polyamide composite reverse osmosis （RO） membrane is easy to be oxidated. N,N＇-Dimethyl-1,3-benzenediamine（DMMPD） as a key functional monomer can be used to prepare the chlorine resistance RO membrane by interfacial polymerization technology. In this work, the DMMPD was synthesized by reduction method with composite reductant NaBH4-I2. The m-phenylenediamine as substrate was first reacted with the acylating agent of formic acid to get the intermediate N, N＇-diformyl-m-phenylenediamine, then the resulting intermediate was reduced by NaBH4-I2 to obtain the final product DMMPD, the synthetic technology was further optimized through orthogonal test, and the proposed mechanism of reduction was discussed. The chemical structures of all products were identified via infrared spectra （IR） , hydrogen nuclear magnetic resonance（ 1H NMR） and mass spectragraph（MS）. This current method for preparing the DMMPD has several advantages, including accessible substrate , mild reaction condition, relatively low cost and high yield.