Amorphous dex-rabeprazole sodium and its preparation method
A technology of rabeprazole sodium and rabeprazole sulfide, which is applied in the field of amorphous dex-rabeprazole sodium and its preparation, can solve the problems of slow human body absorption and poor stability, and achieve low water content , high stability, beneficial to the effect of human body absorption
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Embodiment 1
[0040] 9.0g (0.044mol) L-diethyl tartrate, 12.4g (0.044mol) tetraisopropyl titanate, 8.8g N,N-diisopropylethylamine, 0.03g water and 110g absolute ethanol were added to In a 1000mL three-necked flask, the temperature was raised to 45°C, and the reaction was stirred for 1 hour; cooled to 0°C, 50g (0.146mol) Rabeprazole sulfide was added, and then 180g of cumene hydroperoxide alcohol solution (90g peroxide Hydrogen cumene+90g absolute ethanol), the temperature is controlled to 0~5℃ and reacted for 3 hours.
[0041] Detected by liquid chromatography, the content of rabeprazole sulfide was 1.4%, and the content of peroxide was 1%, and the reaction was terminated. Add 600g of 12wt% potassium hydroxide aqueous solution to the reaction solution, stir at room temperature for 1 hour, wash with 150g of toluene, stand for liquid separation, wash the water layer with 150g of ethyl acetate, stand for liquid separation, add glacial acetic acid to the water layer Adjust the pH to 6-7, add dich...
Embodiment 2
[0043] Take 10 g of dex-rabeprazole prepared in Example 1, add 40 g of absolute ethanol to dissolve it, then add 1.3 g of sodium hydroxide, and stir for 1 hour at room temperature for salt formation reaction. After the completion of the reaction, it was concentrated under reduced pressure at 45°C, and then 40 g of absolute ethanol was added for steaming once to obtain dex Rabeprazole sodium oil.
[0044] 40 g of dichloromethane was added to the oily substance of dextrorotatory rabeprazole sodium and stirred to dissolve to obtain an extract of dextrorotatory rabeprazole sodium. Use coulometric method to detect the moisture content of the extract <0.5%, take 160g of isopropyl ether, heat it to 35~40℃, slowly add the extract dropwise to the isopropyl ether under stirring, and a white solid is precipitated and maintained at 35~40 Stir at ℃ for 3 hours, then lower the temperature to 15-20 ℃, filter, and dry the precipitated white solid under reduced pressure to obtain amorphous dex Ra...
Embodiment 3
[0046] Take 10 g of dexrabeprazole prepared in Example 1, add 50 g of absolute ethanol to dissolve it, then add 1.3 g of sodium hydroxide, and stir for 1 hour at room temperature for salt formation. After the completion of the reaction, it was concentrated under reduced pressure at 50°C, and then 40 g of absolute ethanol was added and steamed once to obtain dex Rabeprazole sodium oil.
[0047] Add 60 g of dichloromethane to the oily substance of dextro-rabeprazole sodium and stir to dissolve to obtain an extract of dex-rabeprazole sodium. Use coulometric method to detect the moisture content of the extract <0.5%, take 200g of isopropyl ether, heat it to 35~40℃, slowly add the extract dropwise to the isopropyl ether with stirring, a white solid is precipitated and maintained at 35~40 Stir at ℃ for 4 hours, then lower the temperature to 15-20 ℃, filter, and dry the precipitated white solid under reduced pressure to obtain amorphous dex Rabeprazole sodium.
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