Method for synthesizing TTZ (thiotriazinone) by using self-made organic base catalyst taking graphene as carrier

Abstract

The invention relates to a method for synthesizing TTZ (thiotriazinone) by using a self-made organic base catalyst taking graphene as a carrier. The method comprises steps as follows: 2-methyl thiosemicarbazide, diethyl oxalate, the self-made base catalyst taking graphene as the carrier and methanol are subjected to a cyclization reaction at 0-60 DEG C to produce sodium TTZ, the graphene carrier is separated through decolorization and filtration, acidification with hydrochloric acid is performed, and TTZ is obtained. The self-made base catalyst taking graphene as the carrier is used, so that the reaction is conducted in a homogeneous reaction system, the reaction yield is increased, the cyclization yield of TTZ is increased to 85% (in terms of 2-methylthiourea) or above, meanwhile, the viscosity of the reaction system is reduced, and the reaction is easy to control; the content of byproduct 1-methyl-5-thiol-1,2,4-triazole-3-methyl carboxylate is controlled at 100 ppm or below, and the product quality is improved; due to increase of the yield, the utilization rate of raw materials is increased, environmental protection investment is reduced, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing a triazine ring using a self-made organic base catalyst with graphene as a carrier. Background technique [0002] Triazine ring (TTZ) is a key intermediate for the synthesis of ceftriaxone sodium, and after synthesizing 7-ACT with 7-ACA, ceftriaxone sodium can be synthesized with DAMA, so it is an important intermediate for the production of ceftriaxone sodium. It plays a key role in the production of ceftriaxone sodium. Ceftriaxone sodium, also known as ceftriaxone, is a landmark third-generation cephalosporin antibiotic (trade name: Rocephine) developed by Roche, Switzerland. It was first listed in Switzerland in 1982 and is the first semi-synthetic Broad-spectrum long-acting cephalosporins are mainly used for infections caused by sensitive bacteria, such as respiratory infections (especially pneumonia), ear, nose and throat inf...

AI Technical Summary

Problems solved by technology

[0007] 1. The material in the reaction system is relatively viscous, the local concentration is uneven, and many by-products are formed, resulting in a low cyclization yield, only 55-65%;

[0008] 2. There are many impurities. The by-product 1-methyl-5-mercapto-1,2,4-triazole-3-carboxylic acid methyl ester is an important impurity of the triazine ring, and the impurity content in market products is about 1000ppm;

[0009] 3. The mother liquor contains a large amount of raw materials or by-products, which are difficult or costly to handle, resulting in high production costs and low yields of triazine rings

Images