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ChemicalBook CAS DataBase List Acipimox
51037-30-0

Acipimox synthesis

9synthesis methods
Synthesis of acipimox: Under cooling and stirring, 78 g of maleic anhydride was dissolved in a solution of 60 ml of chloroform, and 40 ml of 30% hydrogen peroxide was added. After 2 h, 4.8 g of 5-Methyl-2-pyrazinecarboxylic acid was added, and the temperature was kept at 0-5 °C for 2 d. The maleic acid was filtered off. Concentrate to a small volume, add ethyl acetate, and filter to obtain 1.1 g of acipimox, the melting point of which is 178-180 °C.
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Yield:51037-30-0 98.5%

Reaction Conditions:

Stage #1: 2-methylpyrazin-5-carboxylic acidwith hydrogenchloride in water; for 0.5 h;
Stage #2: with peracetic acid in water at 20; for 3 h;Reagent/catalyst;Temperature;

Steps:

1-10; 1-2 Example 1

Take 5-methyl pyridine-2-pyridine 50.0g, add to 100.0ml purified water, add 40.0g of hydrochloric acid, stir 30min, add 38.5g peroxyacetic acid, stir at room temperature 3h, use 5h after reaction The 0% sodium hydroxide solution adjusts the pH to 4.0, the reaction solution cools to 5 degrees C to the asimoxymos crystals, after filtration washing (20 ml), 50 degrees C vacuum drying to obtain asimoxymos yield 98.5%, purity 99.98%.

References:

CN112125857,2020,A Location in patent:Paragraph 0033-0056

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