Preparation method of adefovir dipivoxil
A technology of adefovir dipivoxil and ethyl acetate, applied in the field of drug synthesis, can solve the problems of unfavorable use of physical properties, unfavorable environmental protection, high production cost, etc.
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Embodiment 1
[0035] Synthesis of 9-[2-[[[[bis(trimethylacetoxy)methyl]phosphoryl]methoxy]-ethyl]adenine
[0036] Add 55g of adefovir into the flask, add 200ml of N-methylpyrrolidone, add 160ml of chloromethyl pivalate, 90ml of triethylamine, 65g of tetra-n-butylammonium bromide, heat up to 55-65°C for 3h, The reaction is complete when the main peak area is 60% detected by high-performance liquid phase. Add 700ml of ethyl acetate, stir and dissolve for 30min, filter, and wash with 220ml of ethyl acetate for 3 times until the filter cake is white. The filtrate is washed with saturated saline 550ml* 3 times, discard the water phase, dry the organic phase with 110g of anhydrous sodium sulfate for 2h, filter, remove the anhydrous sodium sulfate, and wash the filter cake with 50ml of ethyl acetate, and concentrate the filtrate under reduced pressure at 40-50°C to light yellow viscous 600ml of diethyl ether was added under stirring at 10-15°C. After crystals were precipitated, it was filtered, wa...
Embodiment 2
[0038] Add 55g of adefovir into the flask, add 200ml of DMF, add 160ml of chloromethyl pivalate, 90ml of triethylamine, 45g of tetra-n-propylammonium bromide, raise the temperature to 55-65°C for 3 hours, and detect it by high performance liquid phase The main peak area is 63% and the reaction is complete. Add 700ml of ethyl acetate, stir and dissolve for 30min, filter, and wash with 220ml of ethyl acetate for 3 times until the filter cake is white, wash the filtrate with saturated saline 550ml*3 times, discard The aqueous phase and the organic phase were dried with 110g of anhydrous sodium sulfate for 2h, filtered to remove the anhydrous sodium sulfate, and washed the filter cake with 50ml of ethyl acetate, and the filtrate was concentrated under reduced pressure at 40-50°C to a light yellow viscous liquid, 10- 600ml of diethyl ether was added under stirring at 15°C, after crystals were precipitated, filtered, washed with 50ml of diethyl ether, and vacuum-dried at 40-50°C for ...
Embodiment 3
[0040] Add 55g of adefovir into the flask, add 200ml of DMSO, add 160ml of chloromethyl pivalate, 90ml of triethylamine, 55g of tetra-n-ethylammonium iodide, heat up to 55-65°C for 5 hours, and detect The main peak area is 65% and the reaction is complete. Add 700ml of ethyl acetate, stir to dissolve for 30min, filter, and wash with 220ml of ethyl acetate for 3 times until the filter cake is white. Wash the filtrate with saturated saline 550ml*3 times, discard The aqueous phase and the organic phase were dried with 110g of anhydrous sodium sulfate for 2h, filtered to remove the anhydrous sodium sulfate, and washed the filter cake with 50ml of ethyl acetate, and the filtrate was concentrated under reduced pressure at 40-50°C to a light yellow viscous liquid, 10- 600ml of diethyl ether was added under stirring at 15°C, after crystals were precipitated, filtered, washed with 50ml of diethyl ether, and vacuum-dried at 40-50°C for 4 hours to obtain 56g of adefovir dipivoxil with a y...
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