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以廉价的肌苷为原料,经过糖基的乙酰化和嘌呤碱基6位羰基的氯代,得到2’,3’,5’-三-O-乙酰基-6-氯嘌呤核苷,然后以二氯甲烷为溶剂,在三氟乙酸酐和四丁基硝酸铵的作用下,在嘌呤2位引入硝基。最后在HCl/Et OH溶液中,完成脱除乙酰基和硝基氯代两步反应,得到2,6-二氯嘌呤核苷,纯度98%(HPLC),总收率63%。考察了硝基来源、氯原子来源和反应规模对收率的影响,且反应规模扩大到200 g规模时,收率无明显下降。
The inexpensive inosine is used as a raw material to obtain 2 ’, 3’, 5’-tri-O-acetyl-6-chloropurine nucleoside through acetylation of glycosyl group and chlorination of 6-carbonyl of purine base, and then With dichloromethane as a solvent, trifluoroacetic anhydride and tetrabutyl ammonium nitrate role in the purine 2-position introduction of nitro. Finally, the two-step reaction of removing acetyl and nitrochloride is completed in HCl / EtOH solution to obtain 2,6-dichloropurine nucleoside with a purity of 98% (HPLC) with a total yield of 63%. The effects of the source of nitro group, the source of chlorine atom and the reaction scale on the yield were investigated. When the reaction scale was enlarged to 200 g, the yield did not decrease obviously.