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腺苷的合成新工艺研究

Study of New Synthetic Technology of Adenosine

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【作者】 杨西宁董春红渠桂荣

【Author】 YANG Xi ning,DONG Chun hong,QU Gui rong (College of Chemistry & Environmental Science,He’nan Normal University,Xinxiang 453002,China)

【机构】 河南师范大学化学与环境科学学院!河南新乡453002

【摘要】 以次黄嘌呤为原料与三氯氧磷反应制得 6 氯嘌呤 ,收率为 90 .0 % ;6 氯嘌呤再与四乙酰核糖缩合、氨解制得腺苷 ,收率分别为 75 .0 %和 6 6 7%。三步反应的总收率为 45 %。实验验证 :缩合反应的最佳温度为 130~ 140℃ ,氨解反应最佳条件为 :用 0℃饱和氨甲醇溶液 ,加热至 10 0℃氨解 10h。产品经TLC、IR、1HNMR和MS确证

【Abstract】 A new synthetic technology of adenosine from hypoxanthine was developed,and the overall yield was 45%.The procedure involved three steps.Firstly,hypoxanthine reacted with phosphorus oxychloride to produce 6 chloropurine in 90.0% yield.Then,adenosine was synthesized from 6 chloropurine and tetraacetylribofuranose by condensation and ammonolysis in 75.0% and 66.7% yields respectively.The optimum conditions of condensation and ammonolysis were that the condensation temprature was 130-140 ℃,and then the product was ammonolyzed for 10 h at 100 ℃ by methanol saturated at 0 ℃ with ammonia.The products were confirmed by TLC,IR,\+1HNMR and MS.

【关键词】 腺苷次黄嘌呤缩合氨解
【Key words】 adenosinehypoxanthinecondensationammonolysis
  • 【分类号】TQ463
  • 【被引频次】20
  • 【下载频次】506
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