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Method for synthesizing crude product of methylcobalamin by using cyanocobalamin

A technology of cyanocobalamin and methylcobalamin, which is applied in the fields of chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problems of long synthesis reaction cycle and affecting synthesis yield, etc., to improve the international market competitiveness, process The effect of simplicity and short production cycles

Active Publication Date: 2017-01-25
NINGXIA KINGVIT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1 In this reaction, sodium borohydride is used as the reducing agent, and methyl iodide is used as the raw material. Different raw materials and reaction solvents are used, which affects the synthesis yield. The highest yield reported in the literature does not exceed 95%.
[0004] 2 The synthesis reaction cycle is longer, generally more than 2.5h

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The effective volume of the synthesis reactor is 5m 3 , add ethanol 2m 3 . Add 50kg of cyanocobalamin, 2.7kg of trimethylsulfoxide iodide, and 0.1kg of cobalt chloride into the reaction kettle respectively, control the stirring speed at 50r / min, and stir for 20min.

[0026] A high-purity nitrogen gas was introduced into the synthesis reactor for protection.

[0027] Add lithium aluminum hydride 10kg in the synthetic reactor.

[0028] The synthesis temperature is controlled at 30° C., the stirring speed is controlled at 40 r / min, and the synthesis reaction time is controlled at 60 min.

[0029] After the synthesis reaction was completed, it was concentrated under reduced pressure, the pressure was controlled at -0.05 MPa, and the temperature was controlled at 40°C. The ethanol was collected to obtain 48.6 kg of crude methylcobalamin, with a synthesis yield of 97.2% and an effective content of the crude product of 94.3%.

Embodiment 2

[0031] The effective volume of the synthesis reactor is 5m 3 , add ethanol 2.1m 3 . Add 47kg of cyanocobalamin, 2.68kg of trimethylsulfoxide iodide, and 0.14kg of cobalt chloride into the reaction kettle respectively, control the stirring speed at 55r / min, and stir for 25min.

[0032] A high-purity nitrogen gas was introduced into the synthesis reactor for protection.

[0033] Add lithium aluminum hydride 10.34kg in the synthetic reactor.

[0034] The synthesis temperature was controlled at 33° C., the stirring speed was controlled at 45 r / min, and the synthesis reaction time was controlled at 65 min.

[0035] After the synthesis reaction was completed, it was concentrated under reduced pressure, the pressure was controlled at -0.06MPa, the temperature was controlled at 42°C, and ethanol was collected to obtain 45.8kg of crude methylcobalamin, with a synthesis yield of 97.4% and an effective content of the crude product of 94.5%.

Embodiment 3

[0037] The effective volume of the synthesis reactor is 5m 3 , add ethanol 2.25m 3 . Add 45kg of cyanocobalamin, 2.66kg of trimethylsulfoxide iodide, and 0.18kg of cobalt chloride into the reaction kettle respectively, control the stirring speed at 60r / min, and stir for 30min.

[0038] A high-purity nitrogen gas was introduced into the synthesis reactor for protection.

[0039] Add lithium aluminum hydride 11.25kg in the synthetic reactor.

[0040] The synthesis temperature was controlled at 35° C., the stirring speed was controlled at 50 r / min, and the synthesis reaction time was controlled at 70 min.

[0041] After the synthesis reaction was completed, it was concentrated under reduced pressure, the pressure was controlled at -0.08MPa, and the temperature was controlled at 45°C. The ethanol was collected to obtain 44kg of crude methylcobalamin, with a synthesis yield of 97.9% and an effective content of the crude product of 94.8%.

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PUM

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Abstract

The invention relates to a method for synthesizing a crude product of methylcobalamin by using cyanocobalamin. The method comprises the process steps of adding the cyanocobalamin, trimethylsulfoxonium iodide and cobalt chloride into an ethanol solution, and carrying out reaction under the condition of stirring; then, under the protection of high-purity nitrogen, adding lithium aluminium hydride for carrying out reaction; after the reaction is finished, carrying out vacuum concentration to obtain the crude product of the methylcobalamin, wherein the effective content reaches 94%, the synthesis total recovery reaches 97%, and the synthesis cycle is controlled within 80min. The method is simple in technology, short in production cycle, low in production cost and beneficial to international market competitiveness of the methylcobalamin.

Description

technical field [0001] The invention belongs to the technical field of vitamin synthesis, in particular to a method for synthesizing crude methylcobalamin by using cyanocobalamin. Background technique [0002] Methylcobalamin is a coenzyme-type vitamin B12 developed by Eisai Co., Ltd. of Japan. It is an anti-anemia drug. Kylation to give methylcobalamin. There are following technical defects in this method: [0003] 1 In this reaction, sodium borohydride is used as the reducing agent, methyl iodide is used as the raw material, and different raw materials and reaction solvents are used, which affects the synthesis yield. The highest yield reported in the literature does not exceed 95%. [0004] 2 The synthesis reaction period is relatively long, generally over 2.5 hours. [0005] 3 The effective content in the crude product shall not exceed 92%. Contents of the invention [0006] The object of the present invention is to overcome the defect in the above-mentioned prior ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H23/00C07H1/00
CPCC07H1/00C07H23/00
Inventor 任勇
Owner NINGXIA KINGVIT PHARMA
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