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Preparation method of high-purity pravastatin 1, 1, 3, 3-tetramethyl butylamine

A technology of tetramethylbutylamine and tetramethylbutylamine wet powder, which is applied in the preparation of organic compounds, the preparation of amino compounds from amines, the preparation of carboxylate, etc., can solve the problem of affecting the accuracy of detection results, low purity, High price and other problems, to achieve the effect of facilitating the promotion and application of industrial scale, improving the purity of the product, and stabilizing the preparation method

Pending Publication Date: 2022-02-11
GUANGDONG BLUE TREASURE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, pravastatin 1,1,3,3-tetramethylbutylamine is usually purchased from the Pharmacopoeia Commission or professional institutions as a primary standard, and the price is relatively high. If it is used for daily detection, the cost is relatively high; On the one hand, pravastatin sodium is hygroscopic. If the purity of pravastatin sodium itself is not high, further moisture absorption will seriously affect the accuracy of the test results.
However, there is currently no technical disclosure on how to prepare high-purity pravastatin 1,1,3,3-tetramethylbutylamine stably and efficiently. Therefore, how to obtain a high-purity and highly stable pravastatin 1, 1,3,3-Tetramethylbutylamine is of great significance to the preparation and detection of statins

Method used

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  • Preparation method of high-purity pravastatin 1, 1, 3, 3-tetramethyl butylamine
  • Preparation method of high-purity pravastatin 1, 1, 3, 3-tetramethyl butylamine
  • Preparation method of high-purity pravastatin 1, 1, 3, 3-tetramethyl butylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] S1. Accurately weigh 50g of pravastatin sodium, add 500mL of purified water pre-cooled to 10°C, and stir until the pravastatin sodium is completely dissolved;

[0043] S2. Add 2 times the volume of butyl acetate pre-cooled to 10°C to S1, add acetic acid solution with a mass concentration of 30% under stirring conditions to adjust the pH to 3.5, and control the time from the addition of the acetic acid solution to the end of the extraction within 15 minutes , keep the solution at 10°C during the extraction process;

[0044] S3. After the extraction is completed, let it stand for 5 minutes, separate the water layer and the butyl acetate layer, add a small amount of water layer to the unseparated middle layer to continue the extraction, and mark the combined butyl acetate layer as extract 1;

[0045] S4. Immediately add 30 mL of 1,1,3,3-tetramethylbutylamine to the extract 1, and stir for 6 minutes;

[0046]S5. Concentrate the solution obtained in S4 under vacuum at 33°C ...

Embodiment 2

[0051] The difference from Example 1 is that the purified water in step S1 is pre-cooled to 5°C, and the rest of the steps are the same as in Example 1;

[0052] In this example, 40.42 g of pravastatin 1,1,3,3-tetramethylbutylamine was obtained with a purity of 99.750%.

Embodiment 3

[0054] The difference from Example 1 is that the acetic acid solution in step S2 adjusts the pH to 4.0, and the rest of the steps are the same as in Example 1;

[0055] In this example, 40.35 g of pravastatin 1,1,3,3-tetramethylbutylamine was obtained with a purity of 99.768%.

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Abstract

The invention belongs to the technical field of pharmacy, and particularly relates to a preparation method of high-purity pravastatin 1, 1, 3, 3-tetramethyl butylamine. The method comprises the following steps: dissolving pravastatin sodium at the temperature of lower than 10 DEG C, performing low-temperature extraction with butyl acetate, then reacting with 1, 1, 3, 3-tetramethyl butylamine, performing vacuum concentration separation, breaking system equilibrium to separate out pravastatin 1, 1, 3, 3-tetramethyl butylamine, and further reacting with 1, 1, 3, 3-tetramethyl butylamine in an acetone solution again to obtain the high-purity pravastatin 1, 1, 3, 3-tetramethyl butylamine. According to the preparation method, the content of isomer impurities and lactonized impurities is greatly reduced, the preparation method is stable and good in repeatability, the purity of the obtained pravastatin 1, 1, 3, 3-tetramethyl butylamine can reach 99.791%, and the preparation method can be used as a quality control method of the pravastatin 1, 1, 3, 3-tetramethyl butylamine.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a preparation method of high-purity pravastatin 1,1,3,3-tetramethylbutylamine. [0002] technical background [0003] Pravastatin Sodium is a 3-hydroxy 3-methylglutaryl coenzyme A reductase (HMG-COA reductase) inhibitor, its structural formula is as follows: [0004] [0005] Pravastatin sodium can effectively reduce serum total cholesterol, low-density lipoprotein and triglyceride, and increase high-density lipoprotein by inhibiting the synthesis of cholesterol in the human body. It was originally used to treat hyperlipidemia and familial hypercholesterolemia, and later adapted to It can slow down the development of atherosclerosis, reduce the occurrence of coronary atherosclerotic lesions and clinical cardiovascular events; taking pravastatin for a long time, no matter whether the patient suffers from coronary heart disease or not, can reduce the incidence of cor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/00C07C69/33C07C209/68C07C211/03
CPCC07C67/00C07C209/68C07C69/33C07C211/03
Inventor 朱敏杰欧金全潘京方锐旋杨樱华
Owner GUANGDONG BLUE TREASURE PHARMA