- Preparation method of pyridoxal 5-phosphate monohydrate
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The invention provides a preparation method of pyridoxal 5-phosphate monohydrate. The preparation method comprises the following steps: 1, first oxidizing pyridoxine hydrochloride to pyridoxal hydrochloride, adding sodium sulfide, then dropwise adding p-ethoxyaniline to the solution, and carrying out a reaction to produce a pyridoxal hydrochloride Schiff base; 2, adding polyphosphoric acid to thepyridoxal hydrochloride Schiff base, performing a stirring reaction, first hydrolyzing polyphosphoric acid and then performing neutralization with an alkali solution to precipitate a large amount of an orange-red solid after the reaction is completed, and filtering and washing the solid to obtain a pyridoxal 5-phosphate Schiff base; and 3, hydrolyzing the pyridoxal 5-phosphate Schiff base with a 2mol/L of alkali solution, adding an organic solvent for extracting and performing liquid separation, adding a strong acid cation exchange resin into the aqueous phase, performing stirring for 1.0 h and then performing vacuum filtration, and performing freeze drying on the filtrate to obtain pyridoxal 5-phosphate monohydrate. The preparation method of pyridoxal 5-phosphate monohydrate is simple inoperation, mild in reaction conditions, relatively high in purity and yield of the final product, and suitable for industrial application, and has relatively good economic benefits.
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Paragraph 0022-0026
(2019/08/20)
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- Synthesis method of pyridoxal phosphate
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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.
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Paragraph 0023; 0024
(2018/03/01)
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- Method for synthesizing pyridoxal phosphate
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The present invention discloses a method for synthesizing pyridoxal phosphate (5'-pyridoxal phosphate). According to the method, pyridoxine hydrochloride is used as a starting material, and is oxidized under mild reaction conditions to obtain a pyridoxal acidic salt, and a phosphate esterification reaction is carried out with a phosphate esterification reagent to obtain pyridoxal phosphate. According to the present invention, the method has advantages of easily-available raw materials, simple route, low toxicity, less side-reaction, easy product separation, easy product characterizing, high yield and the like.
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Paragraph 0019; 0020; 0023; 0026; 0029; 0032; 0035; 0038
(2019/01/08)
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- Gem-Diol and Hemiacetal Forms in Formylpyridine and Vitamin-B6-Related Compounds: Solid-State NMR and Single-Crystal X-ray Diffraction Studies
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The gem-diol moieties of organic compounds are rarely isolated or even studied in the solid state. Here, liquid- and solid-state NMR, together with single-crystal X-ray diffraction studies, were used to show different strategies to favor the gem-diol or carbonyl moieties and to isolate hemiacetal structures in formylpyridine and vitamin-B6-related compounds. The change in position of the carbonyl group in pyridine compounds had a clear and direct effect on the hydration, which was enhanced by trifluoroacetic acid addition. Because of their biochemical importance, vitamin-B6-related compounds were studied with emphasis on the elucidation of the gem-diol, cyclic hemiacetal or carbonyl structures that can be obtained in different experimental conditions. In particular, new racemic mixtures for the cyclic hemiacetal structure from pyridoxal are reported in trifluoroacetate and hydrochloride derivatives.
- Crespi, Ayelén Florencia,Vega, Daniel,Chattah, Ana Karina,Monti, Gustavo Alberto,Buldain, Graciela Yolanda,Lázaro-Martínez, Juan Manuel
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p. 7778 - 7785
(2016/10/13)
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- Kinetisch-spektroskopische Analyse komplizierterer Folgereaktionssysteme
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For certain consecutive reactions with two linearly independent reaction steps a complete kinetic analysis can be performed by using exclusively absorbance-time measurements.If the first reaction step is of pseudo first order, the concentration of the excess component can be varied in different experiments.By means of the "Formal Integration" method the trace and determinant of the kinetic matrix and both eigenvalues may be calculated for each experiment.The concentration dependence of the trace and the determinant may be used to discriminate between different reaction mechanisms and to calculate all rate constants.For the "Formal Integration" method absorbance-time measurements at two or more different wavelengths are required.At these wavelengths all components of the reaction system may absorb with the exception of the excess component.Molar absorptivities do not need to be known.In contrast to other evaluation methods that use the concentration dependence of the eigenvalues, the new method may be applied even if both eigenvalues are of the same order of magnitude.By means of this method the reaction of pyridoxal with histidine in excess is kinetically analyzed.The reaction mechanism is: . - Keywords: Kinetic analysis / Pseudo first order consecutive reactions / Formal Integration / Pyridoxal / Histidine
- Lachmann, Gabriele,Lachmann, Heinrich,Mauser, Heinz
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