Method for scale lercanidipine hydrochloride preparation

A technology of lercanidipine hydrochloride and compound, applied in the direction of organic chemistry, etc., to achieve the effects of high purity, increased safety and high yield

Inactive Publication Date: 2013-06-19
KAMP PHARMA
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  • Abstract
  • Description
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Problems solved by technology

[0007] The present invention aims to overcome the shortcomings of the existing lercanidipine hydrochloride synthesis process, and provides a high-yield, safe, pollution-free, low-cost, and easy-to-operate preparation method for obtaining high-purity lercanidipine hydrochloride, which is suitable for large-scale production production, can meet the requirements of the pharmaceutical field

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  • Method for scale lercanidipine hydrochloride preparation
  • Method for scale lercanidipine hydrochloride preparation
  • Method for scale lercanidipine hydrochloride preparation

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Embodiment Construction

[0026] (1) Dimethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate (DHPCOOCH 3 ) preparation: Take 5g (0.033mol) of m-nitrobenzaldehyde, 8mL (0.072mol) of methyl acetoacetate, 10mL of ethanol, add it into a 100 mL three-necked flask, heat up to 58°C under stirring, and add 4g (0.05 mol) ammonium bicarbonate, 4mL water, stir until no bubbles are produced. Raise the temperature, add zeolite, stir and reflux for 5h. Cool, filter with suction, dry, and weigh 9.4g of yellow solid.

[0027] (2) Preparation of 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester (DHPCOOH): Take 7.0g ( Put 0.02mol) DHPCOOCH3 and 120mL methanol in a 500mL three-neck flask, stir evenly, add 6.4g (0.16mol) NaOH aqueous solution to the reaction flask after cooling, slowly heat to 75°C for reflux reaction for 5h, distill off part of the methanol under reduced pressure, and transfer to the residue Add 400mL of water, add 0.5g of activated carbon,...

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Abstract

The present invention relates to a lercanidipine hydrochloride preparation method, which comprises the following steps that: m-nitrobenzaldehyde, methyl acetoacetate and ammonium bicarbonate are subjected to a reaction in methanol, and cooling and suction filtration are performed to obtain 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid dimethyl ester (DHPCOOCH3); in the presence of methanol, DHPCOOCH3 reacts with a sodium hydroxide solution to obtain 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester (DHPCOOH); and the DHPCOOH, triethylamine, diethyl chlorophosphate, and a side chain of 2,N-dimethyl-N-(3,3-diphenylpropyl)-1-amino-2-propanol form an ester and a hydrochloride in a methylbenzene solution to prepare the lercanidipine hydrochloride, wherein the 2,N-dimethyl-N-(3,3-diphenylpropyl)-1-amino-2-propanol is lercanidipine.

Description

technical field [0001] The invention belongs to the production field of fine chemical products, and in particular relates to a preparation process of lercanidipine hydrochloride, which is used for producing antihypertensive drugs. [0002] Background technique [0003] The chemical name of Lercanidipine hydrochloride is 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)-3,5-pyridinedicarboxylic acid 2-[ N-(3,3-diphenylpropyl)methylamino-1,1-dimethylethyl methyl ester hydrochloride (see figure 1 ), is a highly selective third-generation calcium antagonist, which has the advantages of lipophilicity, high tolerance, short plasma half-life, long-lasting curative effect and low incidence of adverse reactions, and is suitable for moderate and mild hypertension . [0004] As an existing preparation method, in U.S. Patent No. 4,705,797, it is introduced that the compound N-methyl-3,3-diphenylpropylamine is used as a starting material, and 1-chloro-2-methyl-2-propanol in React in xylene ...

Claims

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Application Information

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IPC IPC(8): C07D211/90
Inventor 吴锋陈锋贺莲张静朱敏陈敏周江杨述刘栋华罗玲唐清萍
Owner KAMP PHARMA
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