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报道了一种合成重要的核苷药物中间体2-巯基腺苷的新方法。以2,6-二氯嘌呤和四乙酰核糖为原料,经过缩合、氨解得到2-氯腺苷,继而以DMF为溶剂,和商品化的固体Na2S在90℃反应10 h,以3步和77%的总收率得到标题化合物。考查反应溶剂、原料配比及反应规模对收率的影响。该方法避免了传统方法中需要新制Na2S的苛刻条件,原料廉价易得,且反应规模扩大至100 g时,收率没有降低。
Reported a new method for the synthesis of 2-mercaptoposide, an important nucleoside drug intermediate. Using 2,6-dichloropurine and tetraacetyl ribose as raw materials, 2-chloroadenosine was obtained by condensation and amidolytic reaction, followed by reaction with commercial solid Na2S at 90 ℃ for 10 h with DMF as solvent. The overall yield of 77% yielded the title compound. Examined the reaction solvent, the ratio of raw materials and reaction scale on the yield. The method avoids the harsh conditions that require the new Na2S in the traditional method, the raw materials are cheap and easily obtained, and the yield is not reduced when the reaction scale is expanded to 100 g.