A method for synthesizing symmetrical dinucleoside triphosphate, tetraphosphate and pentaphosphate sodium salt
一种双核苷三磷酸、五磷酸钠的技术，应用在化学仪器和方法、糖衍生物制备、糖衍生物等方向，能够解决副产物多、产物分离困难、反应产率不高等问题，达到简化合成方法、溶解性好、反应活性高的效果
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Embodiment 1
[0012] Synthesis of bis-cytidine triphosphate trisodium salt (6): Cytidine 5'-phosphoryl piperidine triethylammonium salt (2, 100 mg, 0.20mmol), monophosphate bis(tri-n-butylammonium) salt (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 passing through the sodium form of 732 cation exchange resin, 36 mg of biscytidine triphosphate trisodium salt (6) was obtained, with a yield of 58%.
Embodiment 2
[0014] The synthesis of diadenosine triphosphate trisodium salt (7): adenosine 5'-phosphoryl piperidine triethylammonium salt (3, 100 mg, 0.19mmol), monophosphate di(tetrabutylammonium) salt (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. After passing through the sodium form of 732 cation exchange resin, 38 mg of bis-ATP trisodium salt (7) was obtained, with a yield of 60%.
Embodiment 3
[0016] Synthesis of diuridine tetraphosphate tetrasodium salt (9): uridine 5'-phosphoryl piperidine triethylammonium salt (1, 100 mg, 0.20mmol), pyrophosphate tri(tetrabutylammonium) salt (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 (9) 41 mg was obtained after sodium-type 732 cation exchange resin, with a yield of 58%.
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