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A kind of preparation method of indapamide related substance b
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A technology for indapamide and related substances, applied in the field of preparation of indapamide related substance B, can solve the problems such as the preparation method of substance B not found, and achieve the effects of high yield, short reaction period and low energy consumption
Active Publication Date: 2020-12-15
济南同路医药科技发展有限公司
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Problems solved by technology
[0007] Among them, related substance A and related substance C belong to process impurities, and related substance B is both a process impurity and a degradation impurity. Through literature review, no preparation method of related substance B has been found.
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Embodiment 1
[0023] At 80°C, add indapamide (8.0g, 22mmol) to 200ml of water, then add sodium hydroxide to adjust the pH of the system to 9, stir, and bubble with oxygen, the color gradually becomes darker, continue to react for 8h , the color turned dark brown, TLC tracked the completion of the reaction (dichloromethane:ethyl acetate=4:1), then added 500ml of water to dilute, adjusted the pH value of the system to 6 with 6N hydrochloric acid, solids were precipitated, and filtered to obtain the crude compound , recrystallized with methanol to obtain the pure target compound (4.0 g, yield 50%), HPLC purity 98%.
Embodiment 2
[0025] At 70°C, add indapamide (8.0g, 22mmol) into 200ml of water, then add sodium hydroxide to adjust the pH value of the system to 10, stir, and bubble with oxygen, the color gradually becomes darker, continue to react for 8h , the color turned dark brown, TLC tracked the completion of the reaction (dichloromethane:ethyl acetate=4:1), then added 500ml of water to dilute, adjusted the pH value of the system to 6 with 6N hydrochloric acid, solids were precipitated, and filtered to obtain the crude compound , recrystallized with ethanol to obtain the pure target compound (6.0 g, yield 75%), HPLC purity 92%.
Embodiment 3
[0027] At 90°C, add indapamide (8.0g, 22mmol) to 200ml of water, then add sodium hydroxide to adjust the pH of the system to 9, stir, and bubble with oxygen, the color gradually becomes darker, continue to react for 8h , the color turned dark brown, TLC tracked the completion of the reaction (dichloromethane:ethyl acetate=4:1), then added 500ml of water to dilute, adjusted the pH of the system to 6 with 6N hydrochloric acid, solids were precipitated, and filtered to obtain the crude compound , recrystallized with isopropanol to obtain the pure target compound (6.5 g, yield 81%), HPLC purity 88%.
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Abstract
The invention belongs to the technical field of medicines and particularly relates to a preparation method of indapamide related substance B. The method includes: oxidizing indapamide, as a raw material, under alkali condition with an oxidant to prepare the indapamide related substance B. With the indapamide as an initial material, the related substance B is prepared at high yield and purity justthrough one step of oxidization reaction. The method is simple in operation steps and short in reaction period and low in energy consumption. The method reaches more than 50% in yield and more than 80% in HPLC purity. With water being a solvent, the oxidant is gentle in property, is easy to obtain and is low-cost and environment-friendly; especially, when oxygen is used as the oxidant, introduction and generation of other impurities are avoided, so that the method is clean and high-effective.
Description
technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of a related substance B of indapamide. Background technique [0002] Indapamide increases the excretion of sodium and chloride in the urine by inhibiting the reabsorption of sodium in the dilute segment of the renal cortex, and increases the excretion of potassium and magnesium to a certain extent, thereby increasing urine output. Indapamide exhibits significant antihypertensive activity at doses where the diuretic effect is weak. Moreover, its antihypertensive activity has been confirmed in hypertensive patients with functional anemia. [0003] Indapamide tablets have been used clinically for more than 40 years. In foreign countries, the indapamide tablets originally developed by Servier Company were first approved in the Netherlands on June 12, 1974, and then successively approved in Belgium, the United Kingdom, France and other countries. I...
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