Low-energy-consumption easily-industrializable preparation method for high-purity dihydroartemisinic acid

Abstract

The invention specifically relates to a low-energy-consumption easily-industrializable preparation method for high-purity dihydroartemisinic acid, belonging to the field of medicinal chemistry. The preparation method of the invention comprises the following steps of: (1) extraction and concentration; (2) extraction; (3) acidification; (4) extraction; (5) concentration; (6) primary crystallization; (7) decolorization; (8) recrystallization; and 9) drying. According to the preparation method for dihydroartemisinic acid in the invention, heating is not needed in the steps of extraction and concentration, extraction and acidification, operation temperature is room temperature, and heating is required only when reagents are to be recovered, so energy consumption is low; and the preparation method of the invention does not need treatment with a column or additional arrangement of special equipment, so investment is low, operation is simple, and the preparation method is easy to industrialize and promote. The purity of dihydroartemisinic acid prepared by using the preparation method of the invention reaches 99% or above and is as high as 99.9%, and the yield of 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...

AI Technical Summary

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.

Images