二(三氯甲基)碳酸酯“一锅法”合成磺酰脲类除草剂

One-pot Preparation of Sulfonylurea Herbicide with Bis(trichloromethyl) Carbonate

报道了以双(三氯甲基)碳酸酯(俗称三光气、固体光气,简称BTC)为起始原料合成磺酰脲类的方法。通过这些化合物与不同的胺反应,合成了9种新的磺酰脲化合物,并给出了这些化合物的红外光谱、核磁共振氢谱、元素分析等实验数据。原料2-甲氧羰基苯磺酰胺先与BTC反应生成邻甲氧羰基苯磺酰基异氰酸酯,再与2-(N-丁基)氨基-4-二甲胺基-6-甲氧基-1,3,5-均三嗪反应生成磺酰脲类化合物。避免了传统路线的种种缺点,具有收率高、含量高、成本低的特点。以2-甲氧羰基苯磺酰胺计,总收率为91.7%,原药纯度达96.4%。

A method for the preparation of sulfonylurea herbicide applied bis （trichloromethyl） carbonate as starting material was reported. Through the reaction of these compounds with different amines, nine of new organic sulfonylurea compounds had been prepared. The structures of these compounds were confirmed by IR, 1 MR and elemental analysis. Methyl 2-sulfamoyl benzoate reacted with BTC to get methyl 2-methoxycar-bonylsulfamoyl benzoate. The product reacted with 2-（N-butyl） amino-4-dimethamine -6- methoxy -1,3,5-triazine to get sulfonylurea. This preparation method had high yield and good purity, avoided the shortcoming of the isocyanateroute. The total yield was up to 91.7% based on methyl2-sulfamoylbenzoate and the purity was 96.4%.