A kind of synthetic method of psi-6206 intermediate (2,2-dimethyl-[1,3]dioxolan-4-yl)-hydroxyl-carboxylate

Abstract

5‑(2,2‑Dimethyl‑[1,3]dioxolan‑4‑yl)‑3,4‑dihydroxy‑5H‑furan‑2‑one, hydrogen peroxide, and sodium hydroxide solution are used as raw materials , in the medium of water, 50-60 ° C, dropwise add hydrogen peroxide and sodium hydroxide solution at the same time, control the pH between 8-12, after the drop is completed, keep warm for 10 hours until the reaction is complete, add soda to remove excess hydrogen peroxide, Then lower the temperature to 0-10°C, stir for 3 hours, and filter to obtain RKA20 (2,2-dimethyl-[1,3]dioxolane-4-yl)-hydroxy-acetate) filtrate, filter cake for sodium oxalate. The reaction equation is: .

Description

technical field [0001] The invention belongs to the technical field of organic chemistry and relates to technologies such as oxidation, ring opening and alkali hydrolysis of a five-membered heterocyclic ring, in particular to a (2,2-dimethyl-[1,3]dioxolane-4 -Synthetic technology of -base)-hydroxyl-carboxylate. Background technique [0002] According to the synthetic literature of PSI-6206 intermediate (2,2-dimethyl-[1,3]dioxolan-4-yl)-hydroxyl-carboxylate, potassium hydroxide is used as the alkaline hydrolysis Medium, the produced oxalate ions are dissolved in water, then calcium chloride is added to make the oxalate ions turn into calcium oxalate precipitates, and the calcium oxalate is filtered out to obtain an aqueous solution of PSI-6206 intermediate containing a large amount of potassium salt. Because the aqueous solution contains too much potassium salt, the solution is very viscous in the subsequent synthesis, the stirring load is large, there are many side reaction...

AI Technical Summary

Problems solved by technology

Because the aqueous solution contains too much potassium salt, the solution is very viscous in the subsequent synthesis, the stirring load is large, there are many side reactions, and the reaction is not sufficient. The quality of the final crude product is low, the total yield is not high, and the salt content in the generated waste water also very big

This method not only has high production cost, but also has a large amount of three wastes, and the cost of environmental protection treatment is also very high.

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