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Synthesis method of pyridoxal phosphate

A technology of pyridoxal phosphate and synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problems of low yield and complicated preparation method of pyridoxal phosphate. , to achieve the effect of high yield and simple operation

Inactive Publication Date: 2018-02-02
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the problems of complicated preparation method of pyridoxal phosphate and low yield, the present invention provides a synthetic method of pyridoxal phosphate

Method used

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preparation example Construction

[0013] The embodiment of the present invention provides a kind of synthetic method of pyridoxal phosphate, at least comprises the following steps:

[0014] Step 1, using active manganese dioxide as a catalyst, pyridoxine hydrochloride is oxidized to pyridoxal hydrochloride;

[0015] Step 2, performing a condensation reaction of the pyridoxal hydrochloride and N,N-dimethylethylenediamine to obtain a pyridoxal condensate;

[0016] Step 3. Phosphating the pyridoxal condensate with polyphosphoric acid to prepare crude pyridoxal phosphate.

[0017] The method of the present invention provided by the embodiment of the present invention is simple to operate, the raw and auxiliary materials are easy to obtain, and the yield is higher than 70%, which is suitable for industrial production.

[0018] Preferably, in said step 1, the method for oxidizing pyridoxine hydrochloride to pyridoxal hydrochloride is: providing a hydrochloric acid solution of pyridoxine hydrochloride with a concent...

Embodiment 1

[0035] The present embodiment provides a kind of synthetic method of pyridoxal phosphate, comprising the following steps:

[0036] Step 1, prepare pyridoxal hydrochloride

[0037] Dissolve 50g of pyridoxine hydrochloride into 500mL of hydrochloric acid solution with a mass concentration of 30%, then add 80g of active manganese dioxide, stir and heat up to 50°C for reaction. After 24 hours of reaction, the raw materials are completely converted, and naturally cooled to room temperature 20-25°C, vacuum filtration to obtain the filtrate, the filtrate is concentrated under reduced pressure at 60°C until no liquid flows out to obtain concentrate 1, add 200mL methanol to the concentrate 1 and stir evenly, cool down: cool down within 10 hours To 5°C, a turbid solution was obtained, filtered, and the filter cake was dried to obtain 43g of pyridoxal hydrochloride;

[0038] Step 2, preparation of pyridoxal condensate

[0039] Add the 43g of pyridoxal hydrochloride and 25g of N,N-dimet...

Embodiment 2

[0043] The present embodiment provides a kind of synthetic method of pyridoxal phosphate, comprising the following steps:

[0044] Step 1, prepare pyridoxal hydrochloride

[0045] Dissolve 100g of pyridoxine hydrochloride into 1000mL of hydrochloric acid solution with a mass concentration of 15%, then add 200g of active manganese dioxide, stir and heat up to 55°C for reaction. After 28 hours of reaction, the raw materials are completely converted, and naturally cooled to room temperature 20-25°C, vacuum filtration to obtain the filtrate, the filtrate is concentrated under reduced pressure at 60°C until no liquid flows out to obtain concentrate 1, add 400mL ethanol to the concentrate 1 and stir evenly, cooling: cool down within 10 hours To 5°C, a turbid solution was obtained, filtered, and the filter cake was dried to obtain 88g of pyridoxal hydrochloride;

[0046] Step 2, preparation of pyridoxal condensate

[0047] Add the 88g of pyridoxal hydrochloride and 55g of N,N-dimet...

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Abstract

The invention relates to the technical field of chemical synthesis, and concretely discloses a synthesis method of pyridoxal phosphate. The synthesis method of pyridoxal phosphate comprises the following steps: carrying out an oxidation reaction on pyridoxol hydrochloride under the action of active manganese dioxide to prepare pyridoxal hydrochloride; carrying out a condensation reaction on the pyridoxal hydrochloride and N,N-dimethylethylenediamine to obtain a pyridoxal condensate; and carrying out a phosphate esterification reaction on the pyridoxal condensate under the action of polyphosphoric acid to obtain crude pyridoxal phosphate, and purifying and crystallizing the crude pyridoxal phosphate to obtain the pyridoxal phosphate product. The method has the advantages of easily availableraw and auxiliary materials, mild reaction conditions, high yield and environmental protection.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthetic method of pyridoxal phosphate. Background technique [0002] Pyridoxal phosphate (PLP) is a white crystal, chemical name 2-methyl-3-hydroxy-4-formaldehyde-5-hydroxymethyl pyridinium phosphate, is the coenzyme of transaminase and decarboxylase in amino acid metabolism, can promote gluten Amino acid decarboxylation, enhance the production of γ-aminobutyric acid, which is a neuroinhibitory transmitter. It is clinically used as a drug for the treatment of Parkinson's syndrome, which promotes transaminase transamination and increases the content of dopamine in the body. In addition, it can also catalyze a variety of reactions, the common ones are the transamination of α-amino acid and α-keto acid and the decarboxylation of α-amino acid. [0003] The synthesis of PLP has been the focus of many scholars' research since the beginning of its discovery. Gusalus et ...

Claims

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Application Information

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IPC IPC(8): C07F9/58
CPCC07F9/58
Inventor 李腾王凯何连顺李斌水
Owner JING JING PHARMA
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