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Preparation method of acymose

A technology for intermediates and reaction kettles is applied in the field of preparation of the compound axilimus, and can solve the problems of high production cost, difficult industrialized production, low total yield and the like

Active Publication Date: 2005-08-10
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
  • Preparation method of acymose
  • Preparation method of acymose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: the preparation of intermediate I

[0021] 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 residue, and 20% sodium hydroxide solution was used to Adjust the pH to >10, extract with chloroform, and evaporate the solvent after drying. The residue is recrystallized with toluene, filtered with suction, and dried to obtain 177 g of a white solid with a yield of 77%, m.p.105-107°C.

Embodiment 2

[0022] Embodiment 2: the preparation of intermediate II

[0023] 270ml of acetic anhydride, 78g of sodium acetate and 1750ml of glacial acetic acid were added to the reaction kettle, and after stirring for 10 minutes, if the intermediate I was 133g (1.07mol), after reflux reaction for 5 hours, the solvent was first evaporated under reduced pressure, and then the fractions were collected. 151g of intermediate II was obtained with a yield of 85%, b.p.120-123°C / 12mmHg.

Embodiment 3

[0024] Embodiment 3: the preparation of intermediate III

[0025] Intermediate II 64g (0.38mol) and 300ml of 10% sodium hydroxide solution were stirred at room temperature for 24 hours, extracted with ethyl acetate, anhydrous MgSO 4 After drying, it was concentrated to obtain 39g of intermediate III with a yield of 83%, m.p.34-36°C.

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Abstract

A process for preparing Aximosi from 2,5-dimethyl pyrazine includes such steps as oxidizing by H2O2, esterifying by acetic acid anhydride, hydrolyzing in alkaline condition, and oxidizing by potassium permanganate and H2O2.

Description

technical field [0001] The invention relates to a preparation method of the compound acimomus (5-methylpyrazine-2-carboxylic acid-4-oxide). Background technique [0002] Acipimox (Acipimox) is the general name of 5-methylpyrazine-2-carboxylic acid-4-oxide, and its structural formula is: [0003] [0004] Acilimus is a nicotinic acid derivative used to treat hypertriglyceridemia and hypercholesterolemia, and its lipolysis inhibitory activity is 20 times that of nicotinic acid. 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, reduce the level of triglyceride and total cholesterol in the blood, and at the same time increase the amount of high-density lipoprotein-cholesterol, Usually within one month of taking the medicine, the lipid content in the blood can be improved. Therefore, acipimox is a kind of hypolipidemic drug with great market prospect. [0005] J.Org...

Claims

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Application Information

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IPC IPC(8): C07D241/24
Inventor 赵志全
Owner LUNAN PHARMA GROUP CORPORATION
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