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Embodiment 1
[0039] Get 10 grams of esomeprazole sodium crude product, add 6.7% NaHCO respectively 3 3, 3.5, 4 grams of aqueous solution, stirred for 15-20 minutes, added 20 grams of acetonitrile, stirred at 20°C for 16 hours, filtered, washed the filter cake once with acetonitrile, added 280g of acetonitrile to the filtrate with stirring, and heated at 20°C Stir and crystallize for 6 hours, filter, and vacuum-dry at 35±2°C to obtain esomeprazole sodium.
[0040] Different NaHCO 3 The reaction result under the aqueous solution addition condition is shown in the table below:
[0041] Amount added g 3 3.5 4 Get the amount g 5.10 5.25 5.04 ee value % 99.70 99.90 99.70 Content % 99.70 99.80 99.80 Maximum simple % 0.07 0.04 0.06 Sodium content % 99.30 99.50 99.40
Embodiment 2
[0043] Get 10 grams of esomeprazole sodium crude product, first add 6.7% NaHCO 3 3.5 grams of aqueous solution, stirred for 15 to 20 minutes, added 20 grams of acetonitrile, stirred for 16 hours under different temperature conditions, filtered, the filter cake was washed once with acetonitrile, and 320 g of acetonitrile was added to the filtrate under stirring conditions, stirred and crystallized at 28 ° C After 5 hours, filter, and vacuum-dry at 35±2°C to obtain esomeprazole sodium.
[0044] The reaction results under stirring under different temperature conditions are shown in the following table:
[0045] temperature condition ℃ 20 24 28 32 35 Get the amount g 5.13 6.0 5.22 5.15 5.19 ee value % 99.70 99.90 99.73 99.68 99.73 Content % 99.80 99.82 99.75 99.71 99.75 Maximum simple % 0.08 0.03 0.05 0.08 0.07 Sodium content % 99.20 99.70 99.50 99.40 99.45
Embodiment 3
[0047] Get 10 grams of esomeprazole sodium crude product, first add 6.7% NaHCO 3 4 grams of aqueous solution, stirred for 15 to 20 minutes, added different amounts of acetonitrile, stirred at 24°C for 17 hours, filtered, the filter cake was washed once with acetonitrile, and 300g of acetonitrile was added to the filtrate with stirring, crystallized at 26°C After 6 hours, filter, and vacuum-dry at 35±2°C to obtain esomeprazole sodium.
[0048] The results of different acetonitrile additions are shown in the table below:
[0049] The amount of acetonitrile added g 5 12 20 25 30 Get the amount g 5.1 5.2 5.5 5.3 5.2 ee value % 99.70 99.90 99.73 99.68 99.68 Content % 99.70 99.66 99.75 99.74 99.80 Maximum simple % 0.07 0.06 0.04 0.07 0.08 Sodium content % 99.30 99.45 99.60 99.40 99.50
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Abstract
The invention provides a refinement method of esomeprazolesodium, which comprises the following steps: 1. adding a NaHCO3 water solution into an esomeprazolesodium crude product, adding a solvent, stirring and filtering; and 2. adding a solvent into the filtrate obtained in the step 1, stirring to crystallize, filtering to obtain a wet product, and drying the wet product to obtain the esomeprazolesodium product. The method can effectively remove inorganic impurities and organic impurities in the esomeprazole sodium crude product, and is simple to operate and more suitable for sterile workshop production. The obtained esomeprazole sodium has high optical purity. The content of the esomeprazole sodium refined by the method is up to 99.5% or above, the single impurity content is less than 0.1%, and the sodium content is less than 98-102%.
Description
technical field [0001] The invention belongs to the technical field of medicine and relates to a purification method of esomeprazole sodium salt, in particular to a purification method of esomeprazole sodium salt obtained by asymmetric oxidation. Background technique [0002] Common name for 5-methoxy-2-((S)-((4-methoxy-3,5-dimethyl-2-pyridyl)methyl)sulfinyl-1H-benzimidazole sodium It is esomeprazole sodium (Esomeprazolesodium), the left-handed isomer of omeprazole sodium. Its structural formula is as follows: [0003] [0004] Esomeprazole is a new member of proton pump inhibitors. Proton pump inhibitors (protonpumpinhibitor, PPI) covalently bind to gastric parietal cell H, K-ATPase, inhibit the activity of the enzyme and the secretion of gastric acid, and are widely used in gastric cancer. It is effective in the treatment of acid-related diseases such as esophageal refluxdisease and peptic ulcer. Existing PPIs include omeprazole, lansoprazole and pantoprazole, and es...
Claims
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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 姚庆强石秀娟江文峰张媛
Owner INST OF PHARMACY SHANDONG PROV ACAD OF MEDICAL SCI
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