Synthetic process for acipimox

A synthesis process, the technology of methylpyrazine, applied in the field of synthesis process of acipimox, can solve the problems of high impurity content in crude products, lower production efficiency, unstable process, etc., so as to reduce production cost, simplify production process, reduce The effect of the number of crystallization

Inactive Publication Date: 2016-01-06
SICHUAN YIMING PHARMA CO LTD
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Problems solved by technology

However, the above-mentioned process in the prior art not only has the disadvantage of extremely unstable process, but also produces a crude product with high impurity content, which needs to be recrystallized and purified before obtaining the finished acipimox product with the purity specified in the Pharmacopoeia
However, in the actual produ...

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  • Synthetic process for acipimox
  • Synthetic process for acipimox
  • Synthetic process for acipimox

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preparation example Construction

[0027] In the process of studying the preparation process of acipimox, the present inventors discovered unexpectedly through a large number of screening tests: after the reaction mother liquor obtained in the existing acipimox synthesis process is processed by some specific auxiliary agents, Then add activated carbon for decolorization treatment, and a qualified finished product can be obtained through one cooling crystallization. The above process can effectively reduce the number of crystallization times and avoid recrystallization operations, thus greatly simplifying the production process, improving the synthesis yield, and reducing the overall cost.

[0028] Specifically, the present invention provides:

[0029] A synthesis process of acipimox, which comprises:

[0030] 1) In an aqueous solution, under the action of a catalyst, 5-methylpyrazine-2-carboxylic acid and hydrogen peroxide react as shown in the following formula II,

[0031]

[0032] 2) adding an auxiliary...

Embodiment 1

[0056] Add 6.2g (19mmol) of sodium tungstate dihydrate into a 1L reaction flask, add 400ml of water, stir to dissolve, add 1.9g (19mmol) of concentrated sulfuric acid while stirring, and continue to add 204g (1.8mol) of hydrogen peroxide (30%), Stir evenly, add 207.2g (1.5mol) of 5-methylpyrazine-2-carboxylic acid, heat in a water bath to 60°C, keep stirring for 8 hours, add 31.2g (0.3mol) of sodium bisulfite, and continue stirring for 1 hour. Add 12 g of activated carbon, continue to stir for 1 hour, filter while it is hot, cool the filtrate to 4 ° C, keep for 3 hours, filter, and dry the filter cake at 100 ° C for 3 hours to obtain 196.2 g of off-white crystalline powder with a HPLC purity of 99.35%. The rate is 84.9%.

Embodiment 2

[0058] Add 6.2g (19mmol) of sodium tungstate dihydrate into a 1L reaction flask, add 400ml of water, stir to dissolve, add 1.9g (19mmol) of concentrated sulfuric acid while stirring, and continue to add 306g (2.7mol) of hydrogen peroxide (30%), Stir evenly, add 207.2g (1.5mol) of 5-methylpyrazine-2-carboxylic acid, heat in a water bath to 80°C, keep stirring for 4 hours, add 151.2g (1.2mol) of sodium sulfite, continue stirring for 0.5 hours, and add 20g of activated carbon , continue to stir for 1 hour, filter while hot, cool the filtrate to -4 ° C, keep for 3 hours, filter, and dry the filter cake at 80 ° C for 3 hours to obtain 192.2 g of off-white crystalline powder, HPLC purity 99.1%, yield 83.1 %.

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Abstract

The invention provides a synthetic process for acipimox. The synthetic process comprises steps: firstly, 5-methylpyrazine-2-carboxylic acid and hydrogen peroxide are reacted under action of catalysts in an aqueous solution; secondly, an auxiliary agent is added into the solution obtained in the first step, and the auxiliary agent is one selected from sulfite, bisulfate, oxalic acid and oxalate; thirdly, active carbon is added in the solution obtained in the second step and filtering is carried out; fourthly, the solution obtained in the third step is subjected to cooling crystallization and drying, and an acipimox finshed product is obtained. The synthetic process can lower the crystallization frequency effectively, avoids recrystallization operation, raises the yield and lowers the production cost.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a synthesis process of acipimox. Background technique [0002] Acipimox (Acipimox) is a kind of hypolipidemic drug developed and listed by Italian FarmitaliaCarolErba Company in 1985, which can inhibit the release of free fatty acids from adipose tissue, reduce blood very low density lipoprotein and low density lipoprotein, thereby making blood The reduction of triglyceride and cholesterol concentration in the middle can also promote the increase of high-density lipoprotein, so it is mainly used for the treatment of type IIA, IIR, III, IV and V hyperlipoproteinemia. It has the characteristics of strong lipid-lowering effect, less adverse reactions, good tolerance, suitable for long-term medication and the like. In addition, acilimus can also promote glucose metabolism in patients with non-insulin-dependent diabetes mellitus, which is related to lowering blood sugar; and can e...

Claims

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Application Information

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IPC IPC(8): C07D241/24
Inventor 唐良伟雍智全文薪沣闻亚磊滕德刚熊仕萍俞思勇张桂兴邓华蓉张兰
Owner SICHUAN YIMING PHARMA CO LTD
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