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Preparation method of imidapril hydrochloride

A technology of imidapril hydrochloride and a benign solvent, which is applied in the field of preparation of imidapril hydrochloride, can solve the problems of low purity and large amount of impurities, and achieve the effect of simple operation steps and mild conditions

Inactive Publication Date: 2016-11-16
JIANGSU YONGAN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the existing methods for synthesizing imidapril hydrochloride all contain a large amount of impurities and the purity is not high, so it is necessary to provide a new synthetic method for imidapril hydrochloride

Method used

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  • Preparation method of imidapril hydrochloride
  • Preparation method of imidapril hydrochloride
  • Preparation method of imidapril hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1, the preparation of imidapril hydrochloride

[0058] Add 100 g of the compound shown in formula I to a 1 L reaction flask, add 600 mL of 5 mol / L hydrogen chloride in dioxane solution under mechanical stirring, stir the reaction at 20 ° C, and monitor the reaction by HPLC (such as image 3 As shown, the raw material is almost invisible at 25 minutes), the reaction was completed for 8 hours, filtered, and the solid was air-dried at 50° C. to obtain 74 g of imidapril hydrochloride crude product, with a yield of 85%.

[0059] Purification (recrystallization) of imidapril hydrochloride crude product:

[0060] Add 520ml of absolute ethanol to a 2L reaction flask, add 74g of the imidapril hydrochloride crude product prepared above under mechanical stirring, heat to reflux (78°C), stir to dissolve the solid completely, add 520ml of ethyl acetate, and cool to 0°C , crystallized for 3 hours, filtered, and the solid was air-dried at 40° C. to obtain 59 g of purified ...

Embodiment 2

[0068] Embodiment 2, the preparation of imidapril hydrochloride

[0069] Add 200 g of the compound shown in formula I in a 2L reaction flask, add 1200 mL of 5mol / L hydrogen chloride in dioxane solution under mechanical stirring, stir the reaction at 25 ° C, and monitor the reaction by HPLC (such as Figure 4As shown, the raw material is almost invisible at 25 minutes), the reaction was completed for 8 hours, filtered, and the solid was air-dried at 50° C. to obtain 153 g of imidapril hydrochloride crude product, with a yield of 80%.

[0070] Purification (recrystallization) of imidapril hydrochloride crude product:

[0071] Add 600ml of anhydrous methanol to a 3L reaction flask, add 153g of imidapril hydrochloride crude product prepared above under mechanical stirring, heat to reflux (65°C), stir to completely dissolve the solid, add 1200ml of ethyl acetate, and cool to 0°C , crystallized for 3 hours, filtered, and the solid was air-dried at 40° C. to obtain 122 g of purified...

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Abstract

The invention discloses a preparation method of imidapril hydrochloride. The preparation method comprises the following steps: taking an organic solvent solution of hydrogen chloride as a reaction solvent; and reacting a compound as shown in a formula I in the reaction solvent to obtain the imidapril hydrochloride. The organic solvent is ethyl acetate, methyl tertiary butyl ether or dioxane. In the preparation method, yield of preparation steps of the imidapril hydrochloride is stable basically and is about 85%, purification yield of purification steps of the imidapril hydrochloride is about 80%, and therefore, the integral yield of the preparation method can reach 68% or above. The preparation method is gentle in condition and simple in operation steps, and the high-purity imidapril hydrochloride product can be obtained.

Description

technical field [0001] The invention relates to a preparation method of imidapril hydrochloride, which belongs to the field of drug synthesis. Background technique [0002] (4S)-3-[(2S)-2-[(1S)-1-ethoxycarbonyl-3-phenylpropyl]aminopropionyl]-1-methyl-2-oxoimidazoline shown in formula II -4-Carboxylate hydrochloride, also known as imidapril hydrochloride, trade name Dashuang. [0003] [0004] The active metabolite of imidapril hydrochloride, imidapril, can be used for the renin-angiotensin (RA) system in the body with high selectivity, inhibit the generation of angiotensin II, and inhibit the production of sympathetic neurotransmitters and aldosterone. Secreted, thereby reducing peripheral pressure, to achieve the purpose of lowering blood pressure. At present, the existing methods for synthesizing imidapril hydrochloride all contain a large amount of impurities and the purity is not high, so it is necessary to provide a new synthetic method for imidapril hydrochloride....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/062C07K1/02
CPCC07K5/06026
Inventor 康彦龙袁伟锋孙跃军张文腾
Owner JIANGSU YONGAN PHARMA CO LTD
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