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Preparation method of acymose

An intermediate and reaction kettle technology, which is applied in the field of preparation of the compound acipimox, can solve the problems of difficult industrial production, high production cost, and low total yield

Active Publication Date: 2006-11-01
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the total yield of this reaction route is too low, the production cost is too high, it is difficult to realize suitability for industrialized production

Method used

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  • Preparation method of acymose

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 1: Preparation of Intermediate I

[0018] 200g (1.85mol) of 2,5-dimethylpyrazine, 200ml of 30% hydrogen peroxide and 900ml of acetic acid were stirred and reacted at 70°C for 12 hours, the solvent was evaporated under reduced pressure, 500ml of ice water was added to the remainder, and 20% sodium hydroxide solution Adjust pH>10, extract with chloroform, distill off the solvent after drying, recrystallize the residue with toluene, filter with suction, and obtain 177 g of white solid after drying, with a yield of 77%, mp 105-107°C.

Embodiment 2

[0019] Example 2: Preparation of Intermediate II

[0020] Add 270ml of acetic anhydride, 78g of sodium acetate and 1750ml of glacial acetic acid to the reaction kettle. After stirring for 10 minutes, if intermediate I133g (1.07mol) is refluxed for 5 hours, the solvent is evaporated under reduced pressure, and then the fractions are collected. 151g Intermediate II, the yield is 85%, bp120~123°C / 12mmHg.

Embodiment 3

[0021] Example 3: Preparation of Intermediate III

[0022] Intermediate II64g (0.38mol) and 300ml 10% sodium hydroxide solution were stirred and reacted at room temperature for 24 hours, extracted with ethyl acetate, anhydrous MgSO 4 After drying, it was concentrated to obtain 39 g of Intermediate III, with a yield of 83%, m.p. 34-36°C.

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Abstract

The invention discloses a preparation method of acilimus, which uses 2,5-dimethylpyrazine as a starting material, oxidizes with hydrogen peroxide, esterifies with acetic anhydride, and hydrolyzes it under alkaline conditions, then uses permanganic acid Potassium and hydrogen peroxide are oxidized to produce acipimox. The invention improves the yield of acipimox and greatly reduces the production cost by optimizing the reaction conditions and perfecting the synthesis process, and is suitable for large-scale industrial production.

Description

Technical field [0001] The invention relates to a method for preparing the compound acipimox (5-methylpyrazine-2-carboxylic acid-4-oxide). Background technique [0002] Acipimox is the general name of 5-methylpyrazine-2-carboxylic acid-4-oxide, and its structural formula is: [0003] [0004] Acipimox is a niacin derivative used to treat hypertriglyceridemia and hypercholesterolemia, and its lipolysis inhibitory activity is 20 times that of niacin. It can inhibit the release of free fatty acids from adipose tissue, reduce the blood concentration of very low-density lipoprotein and low-density lipoprotein, resulting in a decrease in blood triglycerides and total cholesterol levels, and at the same time can increase the amount of high-density lipoprotein-cholesterol. Usually, the blood lipid content can be improved within one month of taking the medicine. Therefore, acipimox is a promising hypolipidemic drug with market prospects. [0005] J. Org. Chem. 26, 126 (1961) discloses t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/24
Inventor 赵志全
Owner LUNAN PHARMA GROUP CORPORATION
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