Process for preparing high-purity minodronate

A technology of minodronic acid and high purity is applied in the field of preparing high-purity minodronic acid to achieve the effects of improving human health, simple operation and avoiding hip fractures

Inactive Publication Date: 2017-06-13
成都归合科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

What needs to be emphasized is that there is currently no safe and effective radical cure in medicine to help the loose bones return to their original state. Therefore, correct understanding and early prevention are particularly important.

Method used

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  • Process for preparing high-purity minodronate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Such as figure 1 Shown, a kind of technique for preparing high-purity minodronic acid of the present invention comprises the following processing steps:

[0023] (1) Add 100g of 2-aminopyridine to 1000g of methanol, dropwise add 120g of trans-4-oxyl-2-butenoic acid ethyl ester to react, after about 30min, heat to 85±5℃ for reaction, After completion of the reaction, cool to room temperature to generate 2-(imidazo[1,2-a]-3-yl)ethyl acetate, add 1100g of 10% NaOH for hydrolysis, and concentrate to obtain 2-(imidazo[1,2-a ]-3-yl)acetic acid;

[0024] (2) Add 1200g toluene and 150g phosphorous acid to the solution containing 2-(imidazo[1,2-a]pyridin-3-yl)acetic acid, stir and heat to react, then add 420g phosphorus trichloride dropwise to react, cool , to obtain the crude product of minodronic acid, the heating temperature is 50-120°C.

[0025] (3) Add 5000 g of 1 mol / L hydrochloric acid to the solution containing the crude minophosphoric acid, heat to reflux until compl...

Embodiment 2

[0027] A kind of technique for preparing high-purity minodronic acid of the present invention comprises the following process steps:

[0028] (1) Add 92g of 2-aminopyridine to 1000g of absolute ethanol, add 110g of trans-4-oxyl-2-butenoic acid ethyl ester dropwise to react, drop for about 30min, and heat to 85±5°C After the reaction is complete, cool to room temperature to generate 2-(imidazo[1,2-a]-3-yl)ethyl acetate, add 1000g of 10% NaOH for hydrolysis, and concentrate to obtain 2-(imidazo[1,2 -a]-3-yl)acetic acid;

[0029] (2) Add 1000g of toluene and 130g of phosphorous acid to the solution containing 2-(imidazo[1,2-a]pyridin-3-yl)acetic acid, stir and heat for reaction, then add 380g of phosphorus trichloride dropwise for reaction, and cool , to obtain the crude product of minodronic acid, the heating temperature is 110°C to 120°C;

[0030] (3) Add 4600 g of 1 mol / L hydrochloric acid to the solution containing the crude minophosphoric acid, heat to reflux until complet...

Embodiment 3

[0032] A kind of technique for preparing high-purity minodronic acid of the present invention comprises the following process steps:

[0033] (1) Add 85g of 2-aminopyridine to 1000g of anhydrous n-butanol, add 100g of trans-4-oxyl-2-butenoic acid ethyl ester dropwise to react, drop for about 30min, and heat to 85± React at 5°C, after the reaction is complete, cool to room temperature to generate 2-(imidazo[1,2-a]-3-yl)ethyl acetate, add 1000g of 10% NaOH for hydrolysis, and concentrate to obtain 2-(imidazo[1,2-a] ,2-a]-3-yl)acetic acid;

[0034] (2) Add 900g of toluene and 110g of phosphorous acid to the solution containing 2-(imidazo[1,2-a]pyridin-3-yl)acetic acid, stir and heat for reaction, then add 350g of phosphorus trichloride dropwise for reaction, and cool , to obtain the crude product of minodronic acid, the heating temperature is 110°C to 120°C;

[0035] (3) Add 4500 g of 1 mol / L hydrochloric acid to the solution containing the crude minophosphoric acid, heat to re...

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Abstract

The invention discloses a process for preparing high-purity minodronate. The process comprises the following process steps: firstly, carrying out ring formation on trans-4-oxo-2-ethyl crotonate and 2-aminopyridine so as to generate 2-(imidazo[1,2a]-3-yl)ethyl acetate, and carrying out hydrolysis so as to obtain 2-(imidazo[1,2a]-3-yl)acetic acid; secondly, reacting 2-(imidazo[1,2a]-3-yl)acetic acid, phosphorous acid with phosphorus trichloride to generate crude minodronate; and finally, refining crude minodronate with hydrochloric acid to obtain a finished product. High-purity minodronate prepared by virtue of the process can be used for effectively treating osteoporosis, and serious diseases such as hip fracture are avoided.

Description

technical field [0001] The invention relates to the technical field of chemical pharmacy, in particular to a process for preparing high-purity minodronic acid. Background technique [0002] Osteoporosis is a systemic disease characterized by damage to the microstructure of bone tissue, loss of bone mineral composition and bone matrix, bone thinning, decreased number of trabecular bone, increased bone fragility, and increased risk of fracture. Diseases of bone metabolism disorders. Generally divided into two categories, namely primary osteoporosis and secondary osteoporosis. [0003] Foreign statistics show that there are about 200 million people suffering from osteoporosis in the world, of which there are more than 75 million people in the United States, Western Europe and Japan alone. Osteoporosis is recognized as the second largest health killer after cardiovascular disease. Driven by demand, a market of tens of billions of dollars has been formed. The annual cost of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6561A61P19/10
CPCC07F9/6561
Inventor 刘蓉
Owner 成都归合科技有限公司
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