Method for preparing cytosine arabinoside ester by enzyme catalysis
A technology of cytarabine ester and cytarabine, which is applied in the field of biocatalysis and biosynthesis, biomedicine and materials, can solve the problems of few reaction by-products, low substrate utilization rate, low product purity, etc. Fewer products, no need for group protection and deprotection, high conversion rate of substrate
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Embodiment 1
[0019] will contain 0.5g (2.05×10 -3 mol) Cytarabine, 2.10g (1.84×10 -2 mol) vinyl butyrate, 0.1L 10% (v / v) isopropyl ether-pyridine mixed solvent reaction solution was added in a stoppered Erlenmeyer flask, followed by adding 25,000U lipase derived from Candida antarctica (10,000U / g ), placed in a water bath constant temperature oscillator at 30°C and 150rpm under normal pressure to oscillate, and reacted for 3 hours. After separation and purification by silica gel column chromatography, 0.628g of the product cytarabine 5'-butyrate was obtained, with a yield of 97.5%, and the reaction regioselectivity was 99.9% (the concentration of the product cytarabine 5'-butyrate was high. at 99%).
Embodiment 2
[0021] will contain 0.5g (2.05×10 -3 mol) Cytarabine, 45.9g (2.05×10 -1 mol) vinyl laurate, 0.5L 35% (v / v) the reaction liquid of heptane-dimethylformamide mixed solvent joins in the Erlenmeyer flask with stopper, then adds 100,000U lipase (10,000U) derived from Candida antarctica U / g), placed in a water bath constant temperature oscillator at 40°C and 200rpm under normal pressure to oscillate, after 12 hours of reaction, the reaction mixture was filtered to remove enzymes, concentrated by vacuum evaporation, and the concentrated solution was dried in methanol or ethanol or ethyl acetate Recrystallization or separation and purification through silica gel column chromatography to obtain 0.831 g of the product cytarabine 5'-laurate, with a yield of 96.0%, and a reaction regioselectivity of 99.9% (the product cytarabine 5'-lauric acid The ester concentration is above 99%).
Embodiment 3
[0023] will contain 0.5g (2.05×10 -3 mol) Cytarabine, 313g (8.2×10 -1 mol) methyl tetracosanate, 0.5L 35% (v / v) tetrahydrofuran-pyridine mixed solvent reaction solution was added in a stoppered Erlenmeyer flask, followed by adding 400,000U lipase derived from Candida antarctica (10,000U / g ), placed in a water bath constant temperature oscillator at 60°C and 250rpm under normal pressure to oscillate, and reacted for 8 hours. After separation and purification by silica gel column chromatography, 1.16 g of the product cytarabine 5'-tetradecanoic acid ester was obtained, with a yield of 96.0%; the reaction regioselectivity was 99.9% (the product cytarabine 5'-tetracosine Carbonate concentration is above 99%).
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