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A technology of diacerein and synthetic methods, applied in the field of medicine, can solve the problems of high price, high production cost, unstable product quality, etc., and achieve the effects of low production cost, short production cycle and good application prospects
Active Publication Date: 2016-06-01
SUZHOU LEINA PHARMA RES DEV
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Problems solved by technology
Although the method is simple in technology and has few steps, it needs to use a large amount of sodium acetate or zinc trifluoromethanesulfonate with high price, the production cost is high, and the product quality is not stable
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Embodiment 1
[0024] Examples 1-9 The preparation of Examples 1-9 was completed as follows.
[0025] Accurately weigh 100.0-120.0g of rhein, 2.0-2.4g of anhydrous zinc chloride, and 1700-1860g of acetic anhydride into a 3000mL reaction bottle equipped with mechanical stirring, a thermometer and a condenser, and raise the temperature to 85 ~90°C, the heating process takes about 30 minutes, and the reaction is kept at 85-90°C for about 6 hours. After the reaction is completed, the temperature of the reaction solution is lowered to 25-30° C., and it is sucked to dryness. The filter cake was vacuum-dried at 75-80°C (0.09Mpa) for about 15 hours to obtain the crude product of diacerein, and the content and yield were determined.
[0026] The actual feeding, content and yield of Examples 1-9 are shown in Table 3.
[0029] The refining test of embodiment 10 diacerein
[0030] In order to obtain diacerein with better purity, the sample obtained in Implementation 1 was purified once and twice as follows.
[0031] primary refining
[0032] Table 4 Primary Refining Feeding Amount and Proportion
[0033]
[0034] Test method and result:
[0035] In a 3000mL three-necked reaction flask, 130g of diacerein crude product (Example 1), 720g of NMP, and 755g of MEK were sequentially added, and the temperature was raised to 80-85°C under stirring until all solid materials were dissolved. Keep warm at 80-85°C and filter while hot, rinse with 30mL hot MEK.
[0036] Transfer the filtrate and washing liquid into another clean 3000mL reaction bottle, raise the temperature until the solution is clear, slowly cool and crystallize, keep it in the range of 55-60°C for about 40min, then slowly cool down to 0-5°C, at this temperature Insulation crystallization about 2h. After the crystals are fully separ...
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Abstract
The invention discloses a method for preparing diacerein. The method comprises the following steps of: with domestic high-purity parietic acid as an initiating material, acetic anhydride as a solvent and an acylating agent and zinc chloride anhydrous as a catalyst, preparing a coarse diacerein product and performing secondary refining on the prepared coarse diacerein product so as to prepare diacerein crystals. The diacerein prepared by the method is high in yield and purity, and the method is simple in post-processing process, easy to operate and suitable for industrial production.
Description
field of invention [0001] The invention relates to the technical field of medicine, in particular to a method for synthesizing diacerein with high yield. Background of the invention [0002] Diacerein is an osteoarthritis IL-1 inhibitor researched and developed by TRBCHEMEDICA, Switzerland, for the treatment of degenerative joint diseases (osteoarthritis and related diseases). [0003] The synthesis and preparation of diacerein has a history of more than 20 years, and its preparation methods mainly include chemical total synthesis and chemical semi-synthesis. Among them, there are mainly two total chemical synthesis routes, one is to use 3-nitrophthalic anhydride as the starting material, carry out Friedel-Crafts reaction with m-cresol, and then synthesize the intermediate rhubarb through reduction, cyclization and diazotization phenol, chrysophanol is acetylated and oxidized to obtain diacerein (shown in 1); the second is to use juglone and 6-methoxy-4-methyl-2H-pyran-2-on...
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