A kind of recovery method of phosphate in the synthesis of carbapenicillin key intermediate 4-aa

Abstract

A disclosed method for recovering phosphates during synthesis of a carbapenems key intermediate 4-AA comprises: performing reduced-pressure distillation on phosphate wastewater at 80 DEG C or less, and stopping distillation when the total volume is halved, then adding active carbon to decolor and remove color substances and a part of organics, filtering, adjusting pH of the filtrate to 8-8.5 by using phosphoric acid, cooling to 5-10 DEG C, crystallizing for 1 h, filtering to obtain a filter cake, then performing dry pumping at normal temperature for 2 h, discharging the material and analyzing for production recycling. The method can be used in industrialized production, is simple in operation, has substantial environment-protection and economic dual benefits, and accords with the purpose of reducing sewage characteristic factor.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for recovering phosphate in the synthesis of carbapenicillin key intermediate 4-AA. Background technique [0002] Imipenem, panipenem, meropenem, faropenem, ertapenem, biapenem, doripenem and other penem and carbapenem antibiotics are new atypical β-lactams Antibiotics have antibacterial effects on Gram-negative and positive bacteria, aerobic bacteria, and anaerobic bacteria. (3R, 4R)-3-[(R)-1-tert-butyldimethylsiloxyethyl]-4-acetoxy-2-azetidinone (abbreviation: 4-AA) is a synthetic blue Key intermediates of mycelene and carbapenem antibiotics. At present, the main total synthetic routes of 4-AA can be summarized as the following four: [0003] (1) Using chiral 3-hydroxybutyric acid as starting raw material, it is characterized in that the total yield is low and the cost is high; [0004] (2) Using chiral 1,3-butanediol as the starting raw ma...

AI Technical Summary

Problems solved by technology

[0003] (1) Using chiral 3-hydroxybutyric acid as starting raw material, it is characterized in that the total yield is low and the cost is high;

[0004] (2) Using chiral 1,3-butanediol as the starting raw material is a better industrialization route. Japanese companies mainly adopt this route, but there is no domestic production of this raw material, which is not suitable for domestic industrialized large-scale production;

[0005] (3) With 6-APA as the starting raw material, the raw material cost of this route is too high, the reaction conditions are harsh, the pollution is serious, and it is not suitable for industrialized production;

[0006] (4) With L-threonine as the starting raw material, the raw material of this route is convenient and easy to get, the reaction conditions are relatively easy, and it is suitable for industrial production, but the preparation, separation and purification of (2R, 3R)-2,3-epoxybutyric acid (Intermediate A) is very difficult, and a large amount of lead tetroxide and cerium nitrate are used as oxidants, and there are disadvantages such as heavy metal pollution

[0007] In the synthesis invention, due to the use of phosphate as the protective agent of the oxidant, and the amount of phosphate used in the synthesis is relatively large, after the reaction is complete, it will exist in the form of salt in the water, causing the total phosphorus of the discharged wastewater to be too high. Biochemical aerobic-anaerobic treatment is difficult to meet the expected discharge requirements

Direct treatment through the sewage station requires the addition of a large amount of coagulant aids and flocculants, and produces a large amount of phosphorus-containing solid waste, resulting in secondary sewage discharge

At present, there is no good treatment method for inorganic solid waste, and the treatment operation cost is high