【摘要】 鉴于在尿素法合成甲苯-2,4-二氨基甲酸甲酯(TDC)反应中含有大量的中间产物3-氨基-4-甲基苯氨基甲酸甲酯(TMC),因此,建立TMC的分析方法有助于尿素法合成TDC反应研究。首先采用甲苯为溶剂、ZnCl2为催化剂,以2,4-二氨基甲苯和氯甲酸甲酯为原料合成了TMC;提纯后试样的熔程在1℃以内,表明其纯度较高;然后,采用FT-IR、1 H NMR、元素分析、气质联用分析等方法确定了所合成的TMC试样的结构;采用外标法建立了TMC的高效液相色谱定量分析方法,测得其质量浓度在(0.3~1.5)×10-4 g/mL范围内与峰面积呈现良好的线性关系。更多还原

【Abstract】 In the reaction of dimethyl toluene-2,4-carbamate(TDC)synthesis starting from toluene diamine(TDA),urea and methanol,a large amount of methyl 3-amino-4-methyl-N-phenyl carbamate(TMC)is formed as an intermediate.Therefore,the quantitative analysis of TMC will help the research on the synthesis of TDC.In the present work,TMC was synthesized from TDA and methyl chloroformate with toluene as solvent and ZnCl2 as catalyst first.Then the melting range of purified sample was measured within 1 ℃,indicating the purity of the sample is high,and the structure of TMC was determined by means of FT-IR,1H NMR,elemental analysis and GC-MS.Finally,a HPLC method was established to analyze TMC quantitatively.The results showed that a good linear relationship existed between TMC’s peak area and its concentration which was at the range of(0.3-1.5)×10-4 g/mL.更多还原