A kind of Azilsartan synthesis process
A synthesis process, the technology of AQST-1, applied in the direction of organic chemistry, etc., can solve the problems of affecting the efficacy of drugs and low yield, and achieve the effect of improving product yield and purity, high yield and high AQST content
Active Publication Date: 2021-03-26
HAINAN HUALON PHARM
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Problems solved by technology
And existing synthetic Azilsartan, yield is not high, and produces impurity K and can influence drug effect performance, and its structure is as follows:
Method used
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Embodiment 1
[0033] A Sassartan synthetic process, including the following steps:
[0034] (1) AQST-1 synthesis (化 工)
[0035] In the four-mouth flask, hydroxylamine 39.2 g and dimethyl sulfoxide 240 mL, stirred to dissolution, and the system was added to 25 ° C, 65.52 g of sodium bicarbonate, warmed to 50 ° C, stirred for 50 min, and added to the flask (AQST- SM) 20g, temperature rise to 80 ~ 85 ° C, insulation reaction 20 ~ 22h, TLC point plate reaction substantially complete (no significant AQST-SM spots);
[0036]
[0037] After the reaction, it was reduced to room temperature, and 480 ml of water was added dropwise, stirred for 0.5 hours, filtered, filter cake was rinsed with 80 mL of purified water, and filtered to dryness; filter cake was transferred to the flask, plus 160 ml of isopropanol, heated to 60 ~ 65 At ° C, stir salute 45 to 50 min, cool down to room temperature, filtered, filter cakes rinsed with a small amount of isopropyl alcohol, filter it to dry; reduce the wetting plat...
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The invention provides an azilsartan synthesis process which is characterized by comprising the following steps: dissolving hydroxylamine hydrochloride into dimethyl sulfoxide, adding sodium bicarbonate at 20-25 DEG C, increasing the temperature to 45-55 DEG C, performing stirring for 45-60 minutes, further adding AQST-SM, increasing the temperature to 80-85 DEG C, and performing a temperature-keeping reaction for 20-22 hours so as to obtain AQST-1; dissolving the AQST-1 into tetrahydrofuran, dropping DBU (diazabicyclo) at 20-25 DEG C, further adding carbonyl diazole, and performing a reactionfor 1.5-2.5 hours at 20-25 DEG C so as to obtain AQST-3; mixing the AQST-3 with a sodium hydroxide solution, increasing the temperature to 70-75 DEG C, and performing a temperature-keeping reaction for 1-2 hours so as to obtain a crude product of AQST; and adding methanol into the crude product of AQST, increasing the temperature to 60-65 DEG C, performing pulping for 45-50 minutes, reducing thetemperature to the room temperature, performing filtering, bleaching filter cakes by using methanol, performing suction filtration till dryness, and performing vacuum drying, so as to obtain an AQST product. By adopting the azilsartan synthesis process provided by the invention, the AQST product is prepared, the yield is high, the content of AQST is high, the content of impurities is low, the quality of the AQST product is remarkably improved, and the azilsartan synthesis process is well applied to production of high-quality azilsartan tablets.
Description
Technical field [0001] The present invention relates to the field of pharmaceutical synthesis, and Background technique [0002] Azishantan tablets are used to treat high blood pressure and market demand. There is a significant impact on the purity of Azishatan in the Azishantan tablets. The existing synthesis of Azassartan, the yield is not high, and the impurity K will affect the efficacy, the structure is as follows: [0003] [0004] Strive to reduce the impurity content, improve its purity, improve its quality, and improve product yield and improve productivity. Therefore, it is urgent to solve the above technical problems. Inventive content [0005] According to this, the present invention proposes an Azisartan synthetic process to prepare an AQST product, high yield, and high AQST content, and remove impurities B (the structure), significantly reduce impurity K content, improve the quality of AQST product. [0006] [0007] The technical solution of the present invent...
Claims
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IPC IPC(8): C07D413/10
CPCC07D413/10
Inventor 陈益智翟小玲廉洁陈雪君
Owner HAINAN HUALON PHARM