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Improved method for synthesizing mecobalamine

A technology of methylcobalamin and cyanocobalamin, which is applied in the field of improved synthesis of methylcobalamin, can solve problems such as complex synthesis process and complex structure, and achieve the effects of good selectivity, high catalytic activity and small feeding ratio

Pending Publication Date: 2022-08-09
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vitamin B12 was discovered in the 1920s. Early methylcobalamin was isolated and extracted from the fermentation broth of streptomycin. The full chemical synthesis of vitamin B12 was also realized in the 1970s, but its structure is complex and the synthesis process is relatively relatively complex. Complicated, so promotion is not implemented

Method used

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  • Improved method for synthesizing mecobalamine
  • Improved method for synthesizing mecobalamine
  • Improved method for synthesizing mecobalamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The qualitative and quantitative detection method of the reaction substrate is: chromatographic column: ChromCore 120 C18 5um; mobile phase: V (10g / L sodium hydrogen phosphate dodecahydrate solution): V (methanol) = 73.5: 26.5 (phosphoric acid adjusts the pH to 3.5 ); flow rate: 0.8mL / min; detection wavelength: 361nm; column temperature: 40°C; running time: 20min; injection volume: 20uL.

[0039] The qualitative and quantitative detection method of the reaction product is: chromatographic column: ChromCore 120 C18 5um; mobile phase: V (3.1g / L sodium dihydrogen phosphate dihydrate solution): V (acetonitrile)=80:20 (phosphoric acid adjusts pH to 3.5) , and then add 3.76g of sodium 1-hexanesulfonate; flow rate: 1.0mL / min; detection wavelength: 266nm; column temperature: 40°C; running time: 30min; injection volume: 20uL.

[0040]In a dark room and under nitrogen protection, in a 250ml three-neck flask, add 3.0g cyanocobalamin, 0.24g cobalt chloride hexahydrate, 75ml deioniz...

Embodiment 2

[0042] The qualitative and quantitative detection methods and operations of reaction substrates and products are the same as those in Example 1.

[0043] In a dark room and under nitrogen protection, in a 250ml three-neck flask, add 3.0g cyanocobalamin, 0.24g cobalt chloride hexahydrate, 75ml deionized water, stir and heat to 55°C to completely dissolve the solid, and the available illuminance is lower than 36lx red light was used to observe the reaction phenomenon, and keep stirring at 55°C for 20min. Then 0.32 g of 10% Pd / C catalyst was added and the temperature was raised to 75°C. 4.0 g of 80% hydrazine hydrate was added to the reaction solution in the previous step through a constant pressure burette under the condition of an ice bath, the dropwise addition time was 2h, and the reaction time was 3h, during which a condensation reflux device was used. After the reduction reaction was completed, the temperature of the reaction solution was cooled to 35° C., 2.0 ml of methyl...

Embodiment 3

[0045] The qualitative and quantitative detection methods and operations of reaction substrates and products are the same as those in Example 1.

[0046] In a dark room and under nitrogen protection, in a 250ml three-neck flask, add 3.0g cyanocobalamin, 0.24g cobalt chloride hexahydrate, 75ml deionized water, stir and heat to 55°C to completely dissolve the solid, and the available illuminance is lower than 36lx red light was used to observe the reaction phenomenon, and keep stirring at 55°C for 20min. Then 0.36 g of 10% Pd / C catalyst was added and the temperature was raised to 75°C. 4.5g of 80% hydrazine hydrate was added to the reaction solution in the previous step through a constant pressure burette under the condition of an ice bath, the dropwise addition time was 2h, and the reaction time was 3h, during which a condensation reflux device was used. After the reduction reaction was completed, the temperature of the reaction solution was cooled to 35° C., 2.0 ml of methyl ...

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Abstract

The invention relates to a preparation method of mecobalamin, which comprises the following steps: under the protection of inert gas, in a darkroom, adding a catalyst into a mixed aqueous solution of cyanocobalamin and cobalt chloride, and dropwise adding hydrazine hydrate for reduction reaction, the catalyst being Pd / C; and after the reaction is finished, adding methyl iodide into the reaction liquid to perform methylation reaction. The raw materials of the reducing agent are cheap, the requirements of safe production and clean production are met, the reaction conditions are mild, the operation is controllable, and the reduction yield is high.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to an improved method for synthesizing methylcobalamin. Background technique [0002] Methylcobalamin is an endogenous vitamin B12, which exists in the blood and spinal fluid. Compared with vitamin B12, it has a good effect on improving the conduction of neurons. It is used to treat megaloblastic anemia caused by vitamin B12 deficiency. Also used for peripheral neuropathy. Vitamin B12 was discovered in the 1820s. In the early stage, methylcobalamin was isolated and extracted from the fermentation broth of streptomycin. The full chemical synthesis of vitamin B12 was also achieved in the 1970s, but its structure was complex and the synthesis process was relatively low. complex, so no promotion was implemented. However, with the improvement of cyanocobalamin fermentation level, cyanocobalamin has gradually achieved mass production, providing high-quality raw materials for ...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H1/00C07H23/00B01J23/44
CPCC07H1/06C07H1/00C07H23/00B01J23/44Y02P20/584
Inventor 卢定强周晨阳王新仙温涛曲津漉
Owner NANJING UNIV OF TECH