Preparation method of mecobalamin

Abstract

The invention discloses a preparation method of mecobalamin. The preparation method includes the steps: A.dissolving cyanocobalamine, cobalt chloride and trimethylsulfoxonium iodide in deionized water to obtain a liquid to react; B. dissolving sodium borohydride in absolute ethyl alcohol and adding the liquid to react which is obtained from the step A so as to generate reaction; C. adjusting the PH of the solution to 5.0-7.0; D. conducting centrifugation to obtain filtrate; E. conducting vacuum evaporation on the filtrate to obtain a concentrate; and F. absorbing the concentrate with a macroporous resin column and then conducting washing, layer developing and resolution, thus obtaining crystallization stock solution; adding acetone in the crystallization stock solution; and after dynamic and static crystallization, conducting filtration, washing and drying, thus obtaining the finished product of the mecobalamin. In the invention, low-concentration reaction liquid is adopted and by the steps of centrifugation, resin extraction, crystallization and the like, the mecobalamin with high yield, high purity and low cost is obtained; and the preparation method belongs to an industrial preparation method.

Description

technical field [0001] The invention relates to the field of chemical industry and pharmacy, in particular to a method for preparing methylcobalamin. Background technique [0002] Methylcobalamin is one of the vitamin B12 series products. Its chemical name is: cobalt-α-[α-5,6-dimethylbenzimidazolyl]-cobalt-β-methylcobalamin amide, which is an octahedral Cobalamin complex. The molecular formula is: C 63 h 91 CoN 13 o 14 P, molecular weight: 1344.41. Methylcobalamin is dark red crystal or crystalline powder with strong hygroscopicity and easy to decompose when exposed to light. It is one of the two coenzyme active forms of vitamin B12 in the body. Methylcobalamin has good transferability to nerve tissue in the body, promotes nucleic acid, protein, and lipid metabolism through methyl conversion reactions, and repairs damaged nerve tissue. It is a raw material drug and is recorded in the Japanese Pharmacopoeia. [0003] At present, the preparation method of methylcobalami...

AI Technical Summary

Problems solved by technology

[0014] ①Because the first step of its extraction is cooling to reduce the solubility of methylcobalamin and precipitate to obtain the crude product, since methylcobalamin still has a solubility of 8000ug / ml in water at 12°C and has a higher solubility in alcohol, therefore, In the first extraction, about 10% of the yield is lost in the liquid. When using this extraction method, in order to obtain a high yield, it is necessary to use a high-concentration cyanocobalamin reaction solution, which is easily dissolved and incompletely resulting in an incomplete reaction;

[0017] ④The crystallization process of recrystallization is adopted, so that the raw materials added in the synthesis reaction and the by-products of the reaction will be attached and wrapped on the surface and inside of the methylcobalamin crystal, so the product purity is low;

[0018] Method 8 also has the disadvantage of yield loss caused by low-temperature crystallization. In the extraction stage, only simple resin operations are used, and two solvents, methanol and acetone, are introduced in the refining stage, which not only increases the solvent recovery system, but also the high occupation of methanol. Hazards become limiting factors for industrial production