Method for synthesizing symmetric bi-ribonucleoside triphosphate sodium salt, bi-ribonucleoside tetraphosphate sodium salt and bi-ribonucleoside pentaphosphates odium salt
A technology of dinucleoside triphosphate and sodium pentaphosphate, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as difficult product separation, many by-products, and low reaction yield, and achieve dissolution Good properties, simplified synthesis method, and high reactivity
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Embodiment 1
[0012] Biscytidine triphosphate trisodium salt ( 6 ) Synthesis: Cytidine 5'-phosphoryl piperidine triethylammonium salt ( 2 , 100 mg, 0.20 mmol), bis(tri-n-butylammonium) monophosphate (24 mg, 0.08 mmol) and 4,5-dicyanoimidazole (59 mg, 0.50 mmol) were dissolved in dry DMF (2 mL) , 20 o C was reacted for 24 hours. The reaction solution was concentrated, and 3 M aqueous sodium acetate (0.5 mL) was added to the residue, followed by ethanol (50 mL). Centrifuge to obtain the crude product of dicytidine triphosphate sodium salt. Ion-exchange gel column chromatography was eluted linearly with 0.3–0.6 M ammonium bicarbonate buffer solution, and the eluent containing the product solution was combined and lyophilized to obtain biscytidine ammonium triphosphate. After sodium type 732 cation exchange resin, biscytidine triphosphate trisodium salt ( 6 ) 36 mg, yield 58%.
Embodiment 2
[0014] Biadenosine triphosphate trisodium salt ( 7 ) Synthesis: Adenosine 5'-phosphoryl piperidine triethylammonium salt ( 3 , 100 mg, 0.19 mmol), bis(tetrabutylammonium) monophosphate (45 mg, 0.08 mmol) and 4,5-dicyanoimidazole (56 mg, 0.48 mmol) were dissolved in dry DMF (2 mL) , 20 o C was reacted for 24 hours. The reaction solution was concentrated, and 3 M aqueous sodium acetate (0.5 mL) was added to the residue, followed by ethanol (50 mL). Centrifuge to obtain the crude product of diadenosine triphosphate sodium salt. Ion-exchange gel column chromatography was eluted linearly with 0.3–0.6 M ammonium bicarbonate buffer solution, and the eluent containing the product solution was combined and lyophilized to obtain diadenosine triphosphate ammonium salt. Diadenosine triphosphate trisodium salt ( 7 ) 38 mg, yield 60%.
Embodiment 3
[0016] Diuridine tetraphosphate tetrasodium salt ( 9 ) Synthesis: Uridine 5'-phosphoryl piperidine triethylammonium salt ( 1 , 100 mg, 0.20 mmol), tri(tetrabutylammonium) pyrophosphate (72 mg, 0.08 mmol) and 4,5-dicyanoimidazole (71 mg, 0.60 mmol) were dissolved in dry DMF (2 mL) , 20 o C reacted for 20 h. The reaction solution was concentrated, and 3 M aqueous sodium acetate (0.5 mL) was added to the residue, followed by ethanol (50 mL). Centrifuge to obtain diuridine tetraphosphate sodium salt crude product. Ion-exchange gel column chromatography was eluted linearly with 0.3–0.6 M ammonium bicarbonate buffer solution, and the eluate containing the product solution was combined and lyophilized to obtain diuridine ammonium tetraphosphate. Diuridine tetraphosphate tetrasodium salt was obtained after sodium type 732 cation exchange resin ( 9 ) 41 mg, yield 58%.
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