Method for separation and purification of salt during production of 2,4,5-triamino-6-hydroxypyrimidine sulfate

Abstract

The invention provides a method for separating and purifying salts in the 2,4,5-triamino-6-hydroxy pyrimidine sulfate production process. The method comprises the following steps that: guanidine nitrate, ethyl cyanoacetate and sodium methoxide serving as raw materials are subjected to a condensation reaction to generate condensate 2,4-diamino-6-hydroxypyrimidine, methanol and sodium nitrate; the condensate 2,4-diamino-6-hydroxypyrimidine, sodium nitrate and sulfuric acid serving as raw materials are subjected to a nitrosation reaction to generate a nitrosified substance 2,4-diamino-5-nitroso-6-hydroxypyrimidine, sodium sulfate and water. According to the method, firstly, after the condensation reaction, sodium nitrate is separated, and purification is carried out; then, sodium sulfate is separated in the nitrosation reaction, and purification is carried out; and byproducts of industrial sodium nitrate and industrial sodium sulfate meeting the national standard are reclaimed, so that hazard waste output is eliminated, wastewater drainage is reduced, salt content in wastewater is reduced, and process wastewater biological treatment is benefited.

Description

technical field [0001] The invention belongs to the process optimization in the field of synthesis of pharmaceutical intermediates, in particular to the optimization of the process for preparing 2,4,5-triamino-6-hydroxypyrimidine sulfate, the separation and purification of inorganic salts in intermediate products, and recovery as by-products, eliminating The amount of hazardous waste generated reduces the amount of wastewater discharged and eliminates the salt content in wastewater, which is beneficial to the biological treatment of process wastewater. It is an economical, effective, green and environmentally friendly clean production process. Background technique [0002] 2,4,5-Triamino-6-hydroxypyrimidine sulfate (TAHMS) is an important intermediate in the synthesis of broad-spectrum antiviral drug acyclovir and anti-anemia drug folic acid. The preparation process is divided into the following steps: [0003] (1) Condensation (cyclization): Put the guanidine nitrate and ...

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Problems solved by technology

At present, the desalination method of wastewater mainly adopts multi-effect evaporation (mainly three-effect) or MVR (mechanical secondary vapor recompression) technology. These two evaporation technologies have the disadvantages of high one-time investment, high energy consumption and hazardous waste. Large volume and high cost of hazardous waste treatment and disposal

(1) One-time investment: due to the high salt content and strong corrosion of wastewater, the evaporation equipment needs to be made of titanium steel as the main material, and the equipment is expensive to manufacture; (2) Operation energy consumption: three-effect evaporation of 1 ton of water requires about 0.4 steam tons, MVR needs 60 to 100 degrees of electricity to evaporate 1 ton of water, high energy consumption and high operating costs; (3) The residue after the two kinds of evaporation technology evaporates waste water is water-containing waste salt slag, based on a moisture content of 20%, With an annual output of 2,000 tons of 2,4,5-triamino-6-hydroxypyrimidine sulfate, 2,067 tons of waste salt slag is produced, which is disposed of as hazardous waste, and the disposal cost is high

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