A kind of tenofovir preparation method suitable for industrialized production
A technology of tenofovir and its products, which is applied in the field of drug synthesis, can solve the problems affecting the yield of industrialized large-scale production process, demanding filtering equipment, and hindering the crystallization of tenofovir, so as to achieve convenient industrial production, easy operation and reproducibility good sex effect
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[0033] Preparation of tenofovir
[0034] Reaction formula:
[0035]
Embodiment 1
[0037] Feed 20kg of (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine and 160L of acetonitrile. Dissolve at 60°C, add 60kg of trimethylbromosilane dropwise, and react under reflux at 80°C. After the reaction was completed, it was filtered, and the filtrate was concentrated. After the concentration is completed, add 160L of water (the amount of water added: (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine=8:1), let the layers stand, and collect the lower liquid . Add 50% sodium hydroxide to adjust the pH value to ≈3.0, use gradient cooling, first cool down to 20°C for crystallization for 4 hours, then cool down to 10°C for 4 hours, then cool down to 0°C for 8 hours, and stir slowly during the process (stirring speed 100r / min, stirring for 5 minutes every hour). The product was suction filtered, dried, and weighed to obtain tenofovir 10.50kg.
Embodiment 2
[0039] Feed 20kg of (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine and 160L of acetonitrile. Dissolve at 60°C, add 60.00kg of bromotrimethylsilane dropwise, and react under reflux at 80°C. After the reaction was completed, it was filtered, and the filtrate was concentrated. After the concentration is completed, add 120L of water (the amount of water added: (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine=6:1), let the layers stand, and collect the lower liquid . Add 50% sodium hydroxide to adjust the pH value to ≈2.5, use gradient cooling, first cool down to 20°C for crystallization for 4 hours, then cool down to 10°C for 8 hours, then cool down to 0°C for 12 hours, and stir slowly during the process (stirring speed 200r / min, stirring for 5 minutes every hour). Suction filtration, dry, weigh, obtain tenofovir 9.73kg.
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