Preparation method of low-energy consumption easy-industrial production high-purity dihydroartemisinic acid

Abstract

The invention belongs to the field of medicinal chemistry, and particularly relates to a preparation method of low-energy consumption easy-industrial production high-purity dihydroartemisinic acid. The method comprises the following steps: (1) performing extraction concentration; (2) performing extraction; (3) performing acidification; (4) performing extraction; (5) performing concentration; (6) performing primary crystallization; (7) performing decolorization; (8) performing recrystallization; and (9) performing drying. According to the preparation method of the dihydroartemisinic acid provided by the invention, the steps of extraction concentration, extraction and acidification do not need heating, the operation temperature is room temperature, heating is required only when reagents arerecovered, so that the energy consumption is lower; the preparation method does not need column chromatography, does not need to add special equipment, and has smaller investment, simple operation, and easy industrialization and promotion; and the purity of the dihydroartemisinic acid prepared by the preparation method all reaches 99%, the highest purity can reach 99.9%, and the yield of the dihydroartemisinic acid is about 75-80%.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for preparing high-purity dihydroartemisinic acid with low energy consumption and easy industrial production. Background technique [0002] Artemisinin is a new type of antimalarial drug discovered by Mr. Tu Youyou, a famous Chinese pharmacist and winner of the 2015 Nobel Prize in Medicine, which has the advantages of "high efficiency, quick action, and low toxicity". It has special effects. From 1973 when artemisinin was discovered to 2018, in the past few decades, artemisinin and artemisinin derivatives have developed into a large industry with an annual output value of 1.5 billion US dollars, and the price of artemisinin In 2012, the price peaked at 5,800 yuan per kilogram in recent years and then fell all the way to 950 yuan per kilogram in 2016. From 2016 to 2018, the price of artemisinin has been at 950-1200 yuan per kilogram for two years. The price...

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Problems solved by technology

[0003] There are many studies and patents on dihydroartemisinic acid extraction from artemisinin waste oil, but up to now, there are still various deficiencies in the industrial production of dihydroartemisinic acid: such as patent CN103524527A, using Molecular distillation technology is used to extract artemisinic acid and dihydroartemisinic acid, but a single high-content dihydroartemisinic acid cannot be obtained, and the capital required for early equipment investment is relatively large; for example, patent CN103694106A uses alkali extraction and acid precipitation to extract dihydroartemisinic acid Artemisinin, the resulting product is 98.6% detected by HPLC. When used to synthesize artemisinin, because the impurity content is too high, the synthetic artemisinin impurities will be too high, so it cannot be directly used in pharmaceuticals; such as patent CN104262137A using alkaline Dihydroartemisinic acid was extracted by solution ultrasonic extraction, and the content of the obtained product was 72% by HPLC, which was not high and could not be directly used in the synthesis of artemisinin, and there were many problems in the large-scale application of ultrasonic extraction technology at present; For example, the patent CN104230699A utilizes the ion exchange resin method to separate and purify dihydroartemisinic acid, the process is long, the resin is desorbed, the activation process is more complicated, and the waste water containing acid and alkali is more.

[0004] In summary, the current dihydroartemisinic acid extraction process has problems such as low product quality, complicated process route, high cost, special production auxiliary equipment, and environmental hazards, which are not conducive to the industrial production of dihydroartemisinic acid.

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