Method for synthesizing dinucleoside tetraphosphate and P2,P3-(dihalo) methylene dinucleoside tetraphosphate
A technology of dinucleoside tetraphosphate and nucleoside triphosphate, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of low yield and long reaction time, and achieve high yield, even The effect of fast coupling reaction and easy product
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Embodiment 1
[0013] P 1 , P 4 -Diuridine-5′,5′-tetraphosphate tetrasodium salt ( 7 ) Synthesis: Uridine phosphoryl piperidine triethylamine salt ( 1 , 98 mg, 0.2 mmol), uridine triphosphate tri-n-butylamine salt ( 4 , 98 mg, 0.1 mmol) and 4,5-dicyanoimidazole (71 mg, 0.6 mmol) were vacuum-dried in a 25 mL round bottom flask for 2 h. Under the protection of argon, 3.0 mL of dry DMF was added and reacted at 20°C for 30 hours. The reaction solution was concentrated under reduced pressure, and the crude product was obtained after adding sodium acetate aqueous solution (3.0 M, 1.0 mL) and 30 mL ethanol solution for precipitation and centrifugation. After dissolving in deionized water, Sephadex (DEAE-A25) ion-exchange column chromatography to obtain the product triethylamine salt, and then obtained after passing through sodium-type 732 cation-exchange resin P 1 , P 4 - Diuridine-5′,5′-tetraphosphate tetrasodium salt 37 mg, yield 42% as a white solid.
Embodiment 2
[0015] P 1 , P 4 -Diadenosine-5′,5′-tetraphosphate tetrasodium salt ( 9 ) Synthesis: adenosine phosphoryl piperidine triethylamine salt ( 2 , 129 mg, 0.25 mmol), adenosine triphosphate tri-n-butylamine salt ( 5 , 119 mg, 0.1 mmol) and 4,5-dicyanoimidazole (83 mg, 0.7 mmol) were vacuum-dried in a 25 mL round bottom flask for 2 hours. Under argon protection, 4.0 mL of dry NMP was added and reacted at 20°C for 32 hours. Add 30 mL of ether solution to precipitate and centrifuge to obtain the crude product. After dissolving in deionized water, Sephadex (DEAE-A25) ion-exchange column chromatography to obtain the product triethylamine salt, and then obtained after passing through sodium-type 732 cation-exchange resin P 1 , P 4 - Diadenosine-5′,5′-tetraphosphate tetrasodium salt 37 mg, 40% yield, white solid.
Embodiment 3
[0017] P 1 -Adenosine-5′- P 4 -guanosine-5′-tetraphosphate tetrasodium salt ( 11 ) Synthesis: the guanosine phosphoryl piperidine triethylamine salt ( 3 , 129 mg, 0.25 mmol), adenosine triphosphate tri-n-butylamine salt ( 5 , 119 mg, 0.1 mmol) and 4,5-dicyanoimidazole (83 mg, 0.7 mmol) were vacuum-dried in a 25 mL round bottom flask for 2 hours. Under argon protection, 4.0 mL of dry NMP was added and reacted at 20°C for 32 hours. Add 30 mL of ether solution to precipitate and centrifuge to obtain the crude product. After dissolving in deionized water, Sephadex (DEAE-A25) ion-exchange column chromatography to obtain the product triethylamine salt, and then obtained after passing through sodium-type 732 cation-exchange resin P 1 -Adenosine-5′- P 4 -Guanosine-5'-tetraphosphate tetrasodium salt 33 mg white solid, yield 35%.
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