Benfotiamine related substance, preparation method, application and detection method
A technology of benfotiamine and related substances, which is applied in the field of drug impurities and preparation, and can solve problems affecting product quality and other issues
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Embodiment 1
[0029]
[0030] Add phosphoric acid (225g) to the reaction flask, within 100°C, add phosphorus pentoxide (150g) in batches, react at 100-110°C for 1-2h, then add compound 4 (150g) and keep warm until the reaction is complete, then cool down to 45 Add drinking water and acetone at about ℃ and keep stirring for 0.5-1 hour, then add the separated oily substance to the mixture of ethanol and water to crystallize and dry to obtain light yellow compound 3: 166g, the yield is 75%
Embodiment 2
[0032]
[0033] Add 6v of water and compound 3 (1.00eq) to the reaction flask in sequence, control the temperature at 0-15°C, add 30% sodium hydroxide solution dropwise, adjust the pH to 12.5-13.0 and keep stirring for 1 hour. After the system has a large amount of solids precipitated. Control the temperature at -1-6°C, add benzoyl chloride (1.00eq) dropwise, and keep the reaction for 1.5-2.5h. Control the temperature at 0-10°C, adjust the pH to 3.8-4.1 with hydrochloric acid and keep stirring for 3 hours. Filter to obtain compound 2, and the yield is 100% for the next step of feeding.
Embodiment 3
[0035]
[0036] Add water (6v) and compound 2 (1.00eq) to the reaction flask in sequence, control the temperature at 0-15°C, add 30% sodium hydroxide solution dropwise, adjust the pH to 8-9 and keep stirring for 1 hour. After a large amount of solids precipitate out of the system. Control the temperature at -1-6°C, add benzoyl chloride (1.00eq) dropwise, and keep the reaction for 1.5-2.5h. Control the temperature at 0-10°C, adjust the pH to 3.8-4.1 with hydrochloric acid and keep stirring for 3 hours. After filtration, the crude product of compound 1 was obtained, and after air-drying at 50°C, it was crystallized with 3v of methanol and 1v of water to obtain compound C with a yield of 40%. Compound C is carried out hydrogen spectrum detection, and the results are shown in figure 1 .
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