A kind of preparation method of dibutyryl cyclic adenosine phosphate compound and metal salt thereof
A technology of dibutyryl cycloadenosine and cycloadenosine, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of single method of dibutyryl cycloadenosine compounds and their metal salts, etc. , to achieve the effect of high product yield, less by-products, and improved yield and purity
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Embodiment 1 2
[0058] Example 1 Synthesis of calcium dibutyryl cycloadenosine monophosphate
[0059] Weigh 10.0g of adenosine cyclophosphate into a 250mL three-necked flask, add magnetron and 50mL of N,N-dimethylformamide (DMF), stir, then add 35.0mL of n-butyric anhydride and 6.0mL of diisopropylethylamine A white suspension was obtained, and the system was ventilated three times to keep the system in a nitrogen protection state, then heated to 80° C. and stirred for 7 hours to obtain a tan solution. Cool the reaction solution to room temperature (15°C), then pour 10 mL of purified water into the reaction solution, stir for 3 hours, and then use an oil pump (vacuum degree <-0.095MPa) to remove DMF under reduced pressure at 55°C (to no obvious difference). droplets) to obtain an oily substance to be treated. The oily substance to be treated was dissolved in water to 150 mL, firstly extracted with 90% EtOAc (EtOAc:PE=9:1) (30 mL*3), and then extracted with DCM (15 mL*3), and the obtained org...
Embodiment 2 2
[0065] Example 2 Synthesis of calcium dibutyryl cycloadenosine monophosphate
[0066] Weigh 2.0g of adenosine cyclophosphate into a 100mL flask, add magnetron and 30mL of THF, stir, then add 7.0mL of n-butyric anhydride and 3.5mL of diisopropylethylamine to obtain a white suspension, and ventilate three times to keep the system at Under nitrogen protection, then heated to 80°C and refluxed for 42 hours to obtain a brown-green solution. The reaction solution was cooled to room temperature (20°C), 5 mL of purified water was added, and the mixture was stirred for 3 hours. Then the THF was spun off under reduced pressure with a water pump until the oily substance was reached, 30 mL of purified water was added to dissolve the oily substance, the aqueous solution was extracted with 90% EtOAc (EtOAc:PE=9:1) 50 mL*3, and then 20 mL of DCM was used *3 Extraction, the obtained organic phase is discarded. The aqueous phase was then extracted with 50 mL*5 of 90% DCM (DCM:MeOH=9:1), and ...
Embodiment 3 2
[0069] Example 3 Synthesis of calcium dibutyryl cycloadenosine monophosphate
[0070] Weigh 5.0g adenosine cyclophosphate into a 500mL three-necked flask, add magnetron and 150mL pyridine, stir, then add 25.0mL n-butyric anhydride and 2.5mL triethylamine to obtain a white suspension, ventilate three times to keep the system under nitrogen protection state, and then heated to 70 °C in the dark, and stirred for 17 hours to obtain a tan solution. The reaction solution was cooled to room temperature (20° C.), 150 mL of purified water was added, and the mixture was stirred for 2 hours. Then the pyridine was spun off under reduced pressure with a water pump until the oily substance was reached, 50 mL of purified water was added to dissolve the oily substance, the aqueous solution was extracted with 90% EtOAc (EtOAc:PE=9:1) 30 mL*3, and then 30 mL of DCM was used *3 The aqueous solution was extracted, and the resulting organic phase was discarded. The aqueous phase was then extract...
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