Industrial production method of azilsartan
A production method, the technology of candesartan, which is applied in the field of pharmaceutical production, can solve the problems that the cost and safety are not suitable for industrial production, cannot reach the medicinal level, and cannot be industrialized production, so as to achieve high economic value and social benefits, and increase the yield , The effect of reducing impurity B
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[0028] Example 1
[0029] The specific operation steps for the production of Azilsartan are as follows:
[0030] 1. Preparation of the compound of formula III:
[0031]
[0032] Add 4.0kg dimethyl sulfoxide, 2.0kg sodium bicarbonate, 1.4kg hydroxylamine hydrochloride, and heat up to about 42±2°C. The stirring reaction is about 2hr, cooled to 25±5°C, centrifuged, the filter cake is washed with 1.4kg dimethyl sulfoxide, the filter cake is discarded, and the filtrate is directly vacuum pumped into the reactor, and the temperature is raised to 45±2°C and added 1.0kg candesartan C6 Alkyl ester (compound represented by formula IV), the temperature was raised to 92±2°C and the reaction was incubated for 12hr. HPLC confirmed that the raw material was less than 1.0%. Cool down to 40°C and add 3.0kg of tap water dropwise, stop dripping when there is turbidity, cool down in a circulating ice-salt bath (cooling in stages, take 1hr) to 10°C, keep stirring for 2hr, centrifuge to obtain...
Example Embodiment
[0040] Example 2
[0041] The specific operation steps for the production of Azilsartan are as follows:
[0042] 1. Preparation of the compound of formula III:
[0043]
[0044] Add 4.0 kg of N-methylpyrrolidone, 1.0 kg of anhydrous sodium carbonate, and 1.3 kg of hydroxylamine hydrochloride, and the temperature is raised to about 30-40 °C. About 2hr of stirring reaction, be cooled to 30 ± 5 ℃, centrifuge, add 1.0kg N-methyl pyrrolidone to wash filter cake, filter cake is discarded, filtrate is directly vacuum pumped into reactor, be warming up to 45 ± 2 ℃ and add 1.0kg candesartan C6 alkyl ester (compound shown in formula IV), the temperature was raised to 95±5°C and the reaction was incubated for 20hr, and HPLC confirmed that the raw material was less than 1%. Cool down to 40°C and add 3.5kg of tap water dropwise, stop dripping when there is turbidity, cool down in a circulating ice-salt bath (cooling in stages, take 1hr) to 10°C, keep stirring for 2hr, centrifuge to ob...
Example Embodiment
[0052] Example 3
[0053] The specific operation steps for the production of Azilsartan are as follows:
[0054] 1. Preparation of the compound of formula III:
[0055]
[0056] Add 4.0kg of N,N-dimethylacetamide, 1.35kg of potassium bicarbonate and 1.4kg of hydroxylamine hydrochloride, and the temperature is raised to about 30-40°C. The reaction was stirred for about 2hr, cooled to 25±5°C, centrifuged, and 1.0kg of N,N-dimethylacetamide was added to wash the filter cake. Candesartan C6 alkyl ester (compound shown in formula IV), heat up to 102±3°C and keep the reaction for 24hr, and HPLC confirms that the raw material is less than 1%. Cool down to 40°C and add 3.2kg of tap water dropwise, stop dripping when there is turbidity, cool down in a circulating ice-salt bath (cooling in stages, take 1hr) to 10°C, keep stirring for 2hr, centrifuge to obtain wet products, return to the kettle for beating once ( 2.0kg of water), centrifuged and dried to obtain 1.0-1.1kg of wet pro...
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