除草剂噻吩磺隆的合成工艺

The Synthesis Process of Thifensulfuron-methyl

主要探讨了除草剂噻吩磺隆的合成工艺,以丙烯腈为原料经氯化反应得1,2-二氯丙腈,以巯基乙酸为原料在催化剂作用下跟甲醇反应生成巯基乙酸甲酯,1,2-二氯丙腈、巯基乙酸甲酯在甲醇钠作用下环合制得氨基噻吩,氨基噻吩经重氮化、氯磺化、氨化制得3-氨基磺酰基噻吩-2-甲酸甲酯,3-氨基磺酰基噻吩-2-甲酸甲酯跟光气反应生成异氰酸酯后与均三嗪缩合,经处理制得噻吩磺隆。实验结果表明,该工艺路线反应收率高,可达90%左右(以三嗪计),含量为96%,易于控制和处理且三废少。

The paper mainly discusses the process of synthesis of thifensulfuron-methyl. Through chlorination reaction we can obtain 1, 2- two chloroethyl nitrile, using acrylonitrile as raw materials. Mercaptoacetic acid is used as raw material to react with methanol methyl thioglycolate the presence of catalyst; and 1, 2- two chloroethyl nitrile, mercaptoacetic acid methyl ester in the presence of sodium methoxide cyclization of amino thiophene. By diazotization, chlorosulfonatation, ammoniatation and aminothiophene 3 - amino-sulfonyl-2 -methyl 3 - amino-sulfonyl-2 - carboxylic acid methyl ester can be obtained. After reaction with phosgene, isocyanate and mesitylene triazine condensation and treated, thifensulfuron is produced. Experimental results show that the process route reaction yield, up to （triazine total） in an amount of 96%, which is easy to handle and control and about 90%less waste.