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Synthesis method of azilsartan intermediate

A synthesis method and compound technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult wastewater treatment, large amount of water-absorbing agent, etc., and achieve the effects of reduced reaction time, fast reaction speed, and solvent safety and environmental protection

Inactive Publication Date: 2018-03-27
JIANGSU ZHONGBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has high reaction purity, but in actual operation, it is found that the amount of water-absorbing agent used in the reaction is too large, and the waste water generated when adding water to crystallize later is not easy to treat

Method used

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  • Synthesis method of azilsartan intermediate
  • Synthesis method of azilsartan intermediate
  • Synthesis method of azilsartan intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Add 200g of ethylene glycol, 17.4g of hydroxylamine hydrochloride, 26.0g of sodium bicarbonate and 20g of anhydrous sodium sulfate into a 500ml reaction bottle, stir and react at 50°C for 3h, filter, add 15g of compound a to the filtrate, control the temperature at 90°C, pressurize 0.5 ~0.6MPa, stirring reaction for 6~8h, central control until the raw material ≤1.0%, gradient cooling to 20~30℃, stirring and crystallization, filtering, rinsing the filter cake with 20g of absolute ethanol to obtain compound b. Yield 94.3%, purity 99.4%.

Embodiment 2

[0058] Add 200g of ethylene glycol, 22.0g of hydroxylamine hydrochloride, 31.7g of sodium bicarbonate and 20g of anhydrous sodium sulfate into a 500ml reaction bottle, stir and react at 50°C for 3h, filter, add 15g of compound a to the filtrate, control the temperature at 90°C, and pressurize at 0.5 ~0.6MPa, stir and react for 6~8h, centrally control until the raw material ≤ 1%, cool down to 20~30°C, stir and crystallize, filter, and rinse the filter cake with 20g of absolute ethanol to obtain compound b. Yield 90.5%, purity 99.7%.

Embodiment 3

[0060] Add 200g of ethylene glycol, 14.8g of hydroxylamine hydrochloride, 25.4g of sodium bicarbonate and 20g of anhydrous sodium sulfate into a 500ml reaction bottle, stir and react at 50°C for 3h, filter, add 15g of compound a to the filtrate, control the temperature at 90°C, pressurize 0.5 ~0.6MPa, stir and react for 6~8h, centrally control until the raw material ≤ 1%, cool down to 20~30°C, stir and crystallize, filter, and rinse the filter cake with 20g of absolute ethanol to obtain compound b. Yield 93.6%, purity 99.3%.

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Abstract

The invention discloses a synthesis method of an azilsartan intermediate, and belongs to the field of pharmaceutical manufacturing, wherein a compound a is adopted as a start raw material; hydroxylamine hydrochloride is subjected to alkali separation and then reacts with the compound. According to the synthesis method disclosed by the invention, the reaction is fast, the product purity reaches 99%or more, and the yield is 90% or higher; the adopted solvent is safe and environment-friendly, cheap and easily available; moreover, the experimental operation is simple, and the synthesis method issuitable for industrial production.

Description

Technical field: [0001] The invention belongs to the field of medicine manufacture, and in particular relates to a method for synthesizing an important intermediate of angiotensin II receptor antagonist azilsartan. Background technique: [0002] The present invention relates to a kind of 2-ethoxy-1-[[2'-(hydroxyamidino)-biphenyl]-4-yl]methyl-1H-benzimidazole-7-carboxylic acid and its ester ( Process for the preparation of compound b). [0003] [0004] where R is H or C 1 -C 4 Alkyl or benzyl, benzhydryl, trityl. [0005] Azilsartan is a new generation of selective AT1 subtype angiotensin II receptor antagonist (ARBS) antihypertensive drug, which has the advantages of stable blood pressure reduction, long-lasting drug effect, high tolerance, and small side effects , developed by Japan's Takeda Pharmaceutical, was first listed in Japan in January 2012. The drug is the next-generation product of candesartan medoxomil, which can be used alone or in combination with othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D235/26
CPCC07D235/26
Inventor 吴四清蒋海松王红喜吴小刚黄双徐强
Owner JIANGSU ZHONGBANG PHARMA
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