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Synthesis method of risedronate sodium

A technology for risedronate sodium and a synthetic method, which is applied in the field of synthesis, can solve the problems of cumbersome processing and long reaction time, and achieve the effects of simple operation method, easy-to-obtain raw materials, and direct process route

Active Publication Date: 2013-12-04
江苏润安制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has mild conditions, but the reaction time is long and the processing is cumbersome

Method used

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  • Synthesis method of risedronate sodium
  • Synthesis method of risedronate sodium
  • Synthesis method of risedronate sodium

Examples

Experimental program
Comparison scheme
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Embodiment

[0022] Embodiment: Synthesize risedronate sodium according to the following specific steps

[0023] Step 1: Synthesis of LX-2: Add compound LX-1 (10g, 0.085mol) to a 250ml single-necked round bottom flask, add 30ml of methanol, lower the temperature to -15°C, stir for 20min, and pass in dry hydrochloric acid gas, the temperature was kept at -10°C, stirred for 12h, filtered, and distilled under reduced pressure to obtain LX-2 imine salt (11.25g, 0.075mol), with a yield of 88%;

[0024] Step 2: Synthesis of LX-3: Add compound LX-2 (11.25g, 0.075mol) into a microwave reactor, add 20ml of methanol, microwave settings: reaction temperature 100°C, reaction time 3h, filter directly after the reaction, The solvent was distilled under reduced pressure to obtain LX-3 (9.8g, 0.05mol), yield 66%;

[0025] Step 3: Synthesis of LX-4: Add compound LX-3 (9.8g, 0.05mol) into a 500ml single-necked bottle, add toluene (200ml) and heat to 90°C, slowly add phosphorus trichloride (3g, 0.07mol) fo...

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Abstract

The invention discloses a synthesis method of risedronate sodium. Add compound LX-1 and methanol into a round-bottomed flask, cool down to -15°C, feed dry hydrochloric acid gas, react at -10°C, filter, and distill to obtain LX -2 imine salt; add compound LX-2 and methanol into a microwave reactor, the microwave reaction temperature is 100°C, filter after the reaction, and distill the solvent under reduced pressure to obtain LX-3; add compound LX-3 and toluene into a single-necked bottle, Heat to 90°C, add phosphorus trichloride dropwise, cool to 0°C after reaction, pour off toluene, add water to reflux, filter, add ethanol to the filtrate, cool and crystallize, filter, wash, and dry to obtain LX-4; add compound LX-4 Add pure water to a single-necked bottle and heat it to a temperature of 60°C, add dropwise 2mol / L NaOH aqueous solution, cool and crystallize, filter, and dry to obtain risedronate sodium; the process route of the present invention is direct, the raw materials are easy to obtain, the operation is simple, and it is green Environmental protection, no complex reactions, no special reagents required, high yield.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a synthesis method of risedronate sodium. technical background [0002] Risedronate Sodium is a third-generation bisphosphonate drug jointly developed by Procter & Gamble (P&G) and Hoechst Mar ion Roussel. Its tablets were first approved for osteoporosis in October 1999 in Sweden . 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. [0003] There are two main synthetic methods of 3-pyridineacetic acid hydrochloride, the key intermediate of risedronate sodium: Method 1: It is prepared by esterification, reduction, chlorination, cyanation, and hydrolysis with nicotinic acid as the starting material. The method is harsh and uses expensive reducing agents such as lithium aluminum hydride and highly toxic cyanide. Methods Dinicotinic acid was prepared by esterificatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/58
Inventor 顾海成马玉恒王伟滕奇
Owner 江苏润安制药有限公司
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