A kind of preparation method of pyridoxal phosphate intermediate
A technology for pyridoxal phosphate and intermediates, which is applied in the field of preparation of pyridoxal phosphate intermediates, can solve problems such as heavy metal residues in products, environmental pollution, and difficult wastewater treatment, and achieve easy industrialization, simple operation, and increased yield Effect
Active Publication Date: 2019-11-19
兰州东瑞制药有限公司
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Problems solved by technology
[0004] At present, the main reports in the literature use pyridoxine hydrochloride as the starting raw material and oxidize manganese dioxide to obtain pyridoxal. Due to the use of manganese dioxide, a large amount of manganese-containing ions will be produced, and wastewater treatment is difficult, leading to environmental pollution problems.
[0005] Patent CN102617455B describes that pyridoxine and pyridoxine hydrochloride are oxidized in water under the catalytic oxidation system of oxygen source, TEMPO catalyst, inorganic salt and amines ratio to prepare pyridoxal and pyridoxal hydrochloride, and the inorganic Salt and various copper salts will produce a large amount of copper ion wastewater, which is cumbersome to deal with, resulting in environmental pollution problems, and the product may have heavy metal residues
Method used
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Embodiment 1
[0022] Add pyridoxine hydrochloride 10.2g (0.05mol), 0.31g TEMPO, 0.14g sodium nitrite, 0.16g bromine into the reactor, add water, feed 0.2MPa oxygen and keep the pressure, react at room temperature for 2h, add p-amino Anisole was stirred to produce a large amount of yellow solid, which was filtered and dried to obtain Compound I with a yield of 93%.
Embodiment 2
[0024] Add 20.4g of pyridoxine hydrochloride, 0.46g of TEMPO, 0.69g of sodium nitrite, 1.37g of 47% hydrobromic acid into the reactor, add water, feed 0.4MPa of oxygen and keep the pressure, react at room temperature for 2h, add p-aminobenzene Methyl ether was stirred to produce a large amount of yellow solid, which was filtered and dried to obtain compound I with a yield of 95%.
Embodiment 3
[0026] Add 20.4g of pyridoxine hydrochloride, 0.78g of TEMPO, 0.69g of sodium nitrite, 0.20g of 47% hydrobromic acid into the reactor, add water, feed 0.6MPa air and keep the pressure, react at room temperature for 2h, add p-aminobenzene Methyl ether was stirred to produce a large amount of yellow solid, which was filtered and dried to obtain compound I with a yield of 92%.
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The invention relates to a preparation method of a pyridoxal phosphate intermediate. The preparation method comprises the following steps: (1) adding a TEMPO type catalyst, an NO compound, a Br-containing compound and an oxidizing agent or a TEMPO type catalyst, sodium hydrogen carbonate, the Br-containing compound and the oxidizing agent into a compound III or hydrochloride thereof which is taken as a starting raw material in water for carrying out a TEMPO oxidation reaction so as to obtain a compound II, wherein the TEMPO type catalysts are TEMPO or derivatives thereof and TEMPO with fixed forms; (2) after the reaction of the step (1) is finished, adding a compound IV, stirring to produce a great deal of yellow solid, filtering, and drying to obtain a compound I. The preparation route of the preparation method is described in the description. The preparation method provided by the invention has the advantages that the preparation method is simple and convenient to operate, mild, efficient, environment-friendly, easy in realization of industrial production and high in product yield.
Description
technical field [0001] The invention belongs to the technical field of preparation of vitamin derivatives, in particular to a preparation method of a pyridoxal phosphate intermediate. Background technique [0002] Compound I is an important intermediate of pyridoxal phosphate, which is a derivative of vitamin B6 and an active form of vitamin B6 involved in various metabolic reactions of fat, protein and carbohydrate. Pyridoxal phosphate is the coenzyme of many amino acid deaminases and decarboxylases in organisms, and also the coenzyme of transaminases that catalyze amino acid transamination. Pyridoxal phosphate can treat and prevent various diseases such as hypertension, cerebrovascular disease, cardiovascular disease and diabetes. Pyridoxal 5'-phosphate is a drug used to treat tardive dyskinesia. [0003] Wherein, pyridoxal is an important intermediate in the preparation of pyridoxal phosphate, and about the preparation of pyridoxal: [0004] At present, the main report...
Claims
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IPC IPC(8): C07D213/66
CPCC07D213/66
Inventor杨军田陈永生周永泉高飞张楚天张良伟
Owner兰州东瑞制药有限公司