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Preparation method of risedronate sodium

A technology of risedronate sodium and risedronic acid, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of long reaction time, harsh reaction conditions, and reaction steps Avoid multiple problems, achieve the effect of avoiding side reactions, high purity, and less loss

Inactive Publication Date: 2015-05-20
LUOHE MEDICAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the key intermediate for preparing risedronate sodium is 3-pyridine acetic acid hydrochloride, the method for preparing 3-pyridine acetic acid hydrochloride in the prior art has the following technical defects: 1, mostly with nicotinic acid as starting Reactant, reaction step is more, and reaction time is longer, and the separation operation of intermediate is loaded down with trivial details, causes the productive rate of risedronate sodium to be very low; toxic cyanide

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  • Preparation method of risedronate sodium
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  • Preparation method of risedronate sodium

Examples

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Embodiment 1

[0024] A preparation method of risedronate sodium, comprising the steps of:

[0025] (1) 3-pyridineformyl chloride in 3-pyridineformyl chloride hydrochloride is freed.

[0026] When the temperature is 15° C., 3-pyridinecarbonyl chloride hydrochloride is added to a mixture of neutral organic solvent and basic organic solvent. The neutral organic solvent is a mixture of methyl tert-butyl ether, butyl acetate and kerosene in a volume ratio of 5:0.5:10; 5 grams of 3-pyridineformyl chloride hydrochloride are added to every 100 mL of the neutral organic solvent Salt. The basic organic solvent is trioctylamine, and the ratio of trioctylamine to 3-pyridinecarbonyl chloride hydrochloride is 6:1. It was then stirred for 30 minutes and filtered. HCl in 3-pyridineformyl chloride hydrochloride and trioctylamine generate trioctylamine hydrochloride, which is precipitated in solid form. The content of 3-pyridineformyl chloride in the filtrate is detected by high performance liquid chroma...

Embodiment 2

[0041] A preparation method of risedronate sodium, comprising the steps of:

[0042] (1) 3-pyridineformyl chloride in 3-pyridineformyl chloride hydrochloride is freed.

[0043] When the temperature is 15° C., 3-pyridinecarbonyl chloride hydrochloride is added to a mixture of neutral organic solvent and basic organic solvent. The neutral organic solvent is a mixture of methyl tert-butyl ether, ethyl acetate and kerosene in a volume ratio of 3:0.3:10; 5 grams of 3-pyridineformyl chloride hydrochloride are added to every 100 mL of the neutral organic solvent Salt. The basic organic solvent is trioctylamine, and the ratio of trioctylamine to 3-pyridinecarbonyl chloride hydrochloride is 6:1. It was then stirred for 30 minutes and filtered. HCl in 3-pyridineformyl chloride hydrochloride and trioctylamine generate trioctylamine hydrochloride, which is precipitated in solid form. The content of 3-pyridineformyl chloride in the filtrate was detected by high performance liquid chrom...

Embodiment 3

[0058] A preparation method of risedronate sodium, comprising the steps of:

[0059] (1) 3-pyridineformyl chloride in 3-pyridineformyl chloride hydrochloride is freed.

[0060] When the temperature is 15° C., 3-pyridinecarbonyl chloride hydrochloride is added to a mixture of neutral organic solvent and basic organic solvent. The neutral organic solvent is a mixture of methyl tert-butyl ether, propyl acetate and kerosene in a volume ratio of 6:0.8:13; 5 grams of 3-pyridineformyl chloride hydrochloride are added to every 100 mL of the neutral organic solvent Salt. The basic organic solvent is trioctylamine, and the ratio of trioctylamine to 3-pyridinecarbonyl chloride hydrochloride is 6:1. It was then stirred for 30 minutes and filtered. HCl in 3-pyridineformyl chloride hydrochloride and trioctylamine generate trioctylamine hydrochloride, which is precipitated in solid form. The content of 3-pyridineformyl chloride in the filtrate was detected by high performance liquid chro...

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Abstract

The invention discloses a preparation method of risedronate sodium. The preparation method comprises the following steps of: (1) dissociating 3-pyridinecarboxylicacid chloride in 3-pyridinecarboxylicacid chloride hydrochloride; (2) reacting 3-pyridinecarboxylicacid chloride with diazomethane to generate a diazoketone compound represented by a formula (I); (3) generating 3-pyridylacetic acid under the common action of a catalyst and water; (4) adding hydrochloric acid, separating an organic phase from an inorganic phase, and evaporating and concentrating the inorganic phase to obtain 3-pyridylacetic acid hydrochloride; (5) converting 3-pyridylacetic acid hydrochloride into risedronic acid in the presence of phosphorus trichloride and phosphorous acid; and (6) reacting risedronic acid with sodium hydroxide solution to generate risedronate sodium. The preparation method of risedronate sodium disclosed by the invention has the advantages of being few in reaction step, short in reaction time, simple in post-treatment and higher in product yield.

Description

technical field [0001] The present invention and the field of drug synthesis particularly relate to a preparation method of risedronate sodium. Background technique [0002] Osteoporosis is a systemic bone metabolic disease characterized by bone loss and bone structure destruction, and is a common and frequently-occurring disease in the elderly, especially postmenopausal women. Risedronate sodium is a third-generation bisphosphonate drug jointly developed by Procter & Gamble and Hoechst Marion Roussel. Its tablets were first approved for osteoporosis in Sweden in October 1999. In April 2000, the US FDA approved this product for the prevention and treatment of postmenopausal osteoporosis and osteoporosis caused by long-term glucocorticoid treatment. The key intermediate for preparing risedronate sodium is 3-pyridine acetic acid hydrochloride, and the method for preparing 3-pyridine acetic acid hydrochloride in the prior art has the following technical defects: 1, mostly star...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/58
Inventor 何新蕾丁素君睢超霞于栋张会芬
Owner LUOHE MEDICAL COLLEGE
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