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A kind of synthetic method of nitrendipine

A technique of nitrendipine and a synthetic method, which is applied in the field of material synthesis, can solve the problems of reducing the synthesis efficiency of the target product, reducing the purity of the target product, etc., and achieve the effects of excellent solvent performance, improving the purity of the product, and reducing production costs

Active Publication Date: 2021-09-28
赤峰万泽药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The esterification reaction of the product will reduce the synthesis efficiency of the target product, and will produce new impurities to reduce the purity of the target product

Method used

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  • A kind of synthetic method of nitrendipine

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Comparison scheme
Effect test

Embodiment 1

[0023] A kind of synthetic method of nitrendipine of the present embodiment, comprises the following steps:

[0024] S1 adds 750g acetonitrile in the there-necked flask;

[0025] S2 stirred acetonitrile, added nitrendipine acylate 200g, nitrendipine condensate 450g successively;

[0026] S3 slowly heats up and reacts at 75°C for 4.5 hours;

[0027] After the S4 reaction is completed, slowly cool down to 5°C and crystallize for 4-6 hours;

[0028] S5 filters nitrendipine, and washes the filter cake with a small amount of cold methanol-water mixed solution (methanol:water=1:1);

[0029] S6 dried nitrendipine at 70° C. for 6 hours to obtain 530 g of nitrendipine with a yield of 86%.

[0030]

Embodiment 2

[0032] The features of this embodiment that are the same as those of Embodiment 1 will not be described in detail. The features of this embodiment that are different from Embodiment 1 are:

[0033] A kind of synthetic method of nitrendipine of the present embodiment, comprises the following steps:

[0034] S1 adds 600g acetonitrile in the there-necked flask;

[0035] S2 stirs acetonitrile, adds nitrendipine acylate 80g, nitrendipine condensate 180g successively;

[0036] S3 slowly heats up and reacts at 80°C for 4.5 hours;

[0037] After the S4 reaction is completed, slowly cool down to 0°C and crystallize for 4-6 hours;

[0038] S5 filters nitrendipine, and washes the filter cake with a small amount of cold methanol-water mixed solution (methanol:water=1:1);

[0039] S6 Dry the nitrendipine at 80° C. for 6 hours.

Embodiment 3

[0041] The features of this embodiment that are the same as those of Embodiment 1 will not be described in detail. The features of this embodiment that are different from Embodiment 1 are:

[0042] A kind of synthetic method of nitrendipine of the present embodiment, comprises the following steps:

[0043] S1 adds 600g acetonitrile in the there-necked flask;

[0044] S2 stirs acetonitrile, adds nitrendipine acylate 120g, nitrendipine condensate 270g successively;

[0045] S3 heats up slowly and reacts at 78°C for 4.5 hours;

[0046] After the S4 reaction is completed, slowly cool down to 2°C and crystallize for 4-6 hours;

[0047] S5 filters nitrendipine, and washes the filter cake with a small amount of cold methanol-water mixed solution (methanol:water=1:1);

[0048] S6 Dry the nitrendipine at 75° C. for 6 hours.

[0049] Because alcohols are used as reaction solvents, the nitrendipine synthesized after the reaction does not reach the Pharmacopoeia standard, and secondar...

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Abstract

The invention relates to a synthesis method of nitrendipine, which comprises the following steps: heating a reactant in a reaction solvent to react to synthesize nitrendipine; cooling down after the reaction, filtering the nitrendipine to dry, and recovering the reaction solvent; The reaction solvent is acetonitrile. The present invention uses the reaction solvent acetonitrile, which does not undergo esterification reaction with the product, avoids the generation of impurities in the synthesis process, and improves the purity of the product of the synthesis reaction; the impurities produced by the reaction are dissolved in the reaction solvent, and nitrendipine is separated out by cooling down, while The impurity will not be separated out, and the effect of purifying the synthesized nitrendipine can be achieved; the reaction solvent acetonitrile can be purified by various methods, and after purification, it can still be used as a reaction solvent to reduce the synthesis cost.

Description

technical field [0001] The invention relates to the technical field of substance synthesis methods, in particular to a synthesis method of nitrendipine. Background technique [0002] Alcohols are a class of polar organic compounds containing hydroxyl groups. Alcohol solvents are all polar solvents, the main varieties are ethanol, isopropanol, n-butanol. Because alcohol solvents have the characteristics of being miscible with various solvents such as water, ether, chloroform, esters and hydrocarbons. Among them, ethanol is a good solvent, which can dissolve many inorganic substances and many organic substances, so ethanol is often used to dissolve plant pigments or medicinal ingredients therein, and ethanol is also commonly used as a solvent for reactions, so that the participants in the reaction Both organic and inorganic substances can be dissolved, increasing the contact area and increasing the reaction rate. The solubility and volatility of isopropanol are similar to t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/90
CPCC07D211/90
Inventor 臧晓明赵凯滕英镡
Owner 赤峰万泽药业股份有限公司
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