Novel synthesis method of hexazinone

Abstract

The invention discloses a novel synthesis method of hexazinone. The method comprises the steps of utilizing guanidine to react with an auxiliary material A to prepare ethylguanidyl formate under the condition of using toluene as a solvent and adding an acid binding agent; after removing water through layering and distillation, adding cyclohexylamine to react with ethylguanidyl formate under the action of a catalyst to prepare hexazinone, wherein the mass amount of cyclohexylamine is equal to that of guanidine. According to the method, the occurrence of a cyclization side reaction is avoided, energy is saved, the consumption is low, and the operation is easy; compared with current synthesis methods, the method has the advantages that the process safety is high, the operability is high, rectification is omitted, and a good application value is obtained.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a new method for synthesizing hexazinone. Background technique [0002] At present, the synthesis method of hexazinone on the market mainly refers to U.S. patents US4178448 and US4150225, which use a strong base as a catalyst for triazine cyclization, so that the alcohol generated by the cyclization is easily exchanged with the dimethylamine group of hexazinone, and side reactions occur , affecting the yield. Its main methods include the following: [0003] 1. Introduce more than equivalent dimethylamine to inhibit the shedding of dimethylamine. The gas dimethylamine used in this method has a large safety hazard. After adding water to remove it, the ammonia nitrogen and total nitrogen in the wastewater are difficult to handle, and the method does not Side reactions cannot be completely suppressed, and about 10% of side reactions still occur. [0004] 2. The alcohol gene...

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Problems solved by technology

[0003] 1. Introduce more than equivalent dimethylamine to inhibit the shedding of dimethylamine. The gas dimethylamine used in this method has a large safety hazard. After adding water to remove it, the ammonia nitrogen and total nitrogen in the wastewater are difficult to handle, and the method does not Side reactions cannot be completely suppressed, and about 10% of side reactions still occur

[0004] 2. Remove the alcohol generated by the reaction in time. This method requires high equipment, is difficult to operate, and has high production costs.

[0005] At the same time, there is also a method for synthesizing hexazinone using phosgene as a raw material, but its safety hazard is relatively large, and the rectification removes the alcohol generated by the reaction. The equipment is complicated and the energy consumption is large.

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