Method for purifying acipimox
A technology of acipimox and purification method, which is applied in the direction of organic chemistry, can solve the problem of low purity of acipimox, and achieve the effects of cost saving, high purification yield and simple operation method
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Embodiment 1
[0039] 1. Preparation of crude acipimox:
[0040] Add 10g of sodium tungstate to 200mL of purified water under stirring, add 110g of 30% hydrogen peroxide after the solid is dissolved, slowly add sulfuric acid dropwise to adjust the pH to 1~2 after the addition is complete, and after stirring for 1 hour, add 5-methylpyrazine- 70g of 2-carboxylic acid, heated to 60-70°C, reacted for 20h, cooled to 0-5°C, continued to stir for 1-2h, and filtered with suction to obtain a pale yellow solid, which was dried to obtain 54.7g of crude acipimox with a purity of 94.813 %.
[0041] 2. Purification of Crude Acipimus
[0042] At room temperature, 20 g (0.13 mol) of crude acipimox was added into 400 mL of purified water under stirring, and 10% sodium hydroxide solution was slowly added dropwise to the system to adjust the pH to 9-10. At this time, the solids were completely dissolved, and 21.65 g (0.195 mol) of anhydrous calcium chloride was added, and the mixture was stirred for 30 minut...
Embodiment 2
[0044] 1. Preparation of acipimox crude product: as in Example 1
[0045] 2. Purification of Crude Acipimus
[0046]At room temperature, 20 g (0.13 mol) of crude acipimox was added into 400 mL of purified water under stirring, and 10% sodium hydroxide solution was slowly added dropwise to the system to adjust the pH to 9-10. At this time, the solids were completely dissolved, and 14.43 g (0.13 mol) of anhydrous calcium chloride was added, and the mixture was stirred for 30 minutes, cooled to 0-5° C., and a large amount of solids gradually precipitated. Stirring was continued for 2h, and a light yellow solid was obtained by suction filtration. Add all the solids into 106 g of 20% sodium carbonate aqueous solution (sodium carbonate, 0.20 mol) in mass fraction, raise the temperature to 60°C, stir for 2 hours, cool in an ice-water bath to 0-5°C, and filter with suction, and adjust the pH of the filtrate to 1 with concentrated hydrochloric acid. ~2, stirred at 0~5°C for 2 hours, ...
Embodiment 3
[0048] 1. Preparation of acipimox crude product: as in Example 1
[0049] 2. Purification of Crude Acipimus
[0050] At room temperature, 20 g (0.13 mol) of crude acipimox was added into 400 mL of purified water under stirring, and 10% sodium hydroxide solution was slowly added dropwise to the system to adjust the pH to 9-10. At this time, the solids were completely dissolved, and 28.86g (0.26mol) of anhydrous calcium chloride was added, and the mixture was stirred for 1 hour, cooled to 0-5°C, and a large amount of solids gradually precipitated. Stirring was continued for 2h, and a light yellow solid was obtained by suction filtration. Add all the solids into 106 g of 20% sodium carbonate aqueous solution (sodium carbonate, 0.20 mol) in mass fraction, raise the temperature to 55°C, stir for 2 hours, cool in an ice-water bath to 0-5°C, and filter with suction, and adjust the pH of the filtrate to 1 with concentrated hydrochloric acid. ~2, stirred at 0~5°C for 2 hours, filtere...
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