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。
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 °C, and then the product was ammonolyzed for 10 h at 100 °C by methanol saturated at 0 °C with ammonia. The products were confirmed by TLC, IR, 1HNMR and MS.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2001年第6期317-318,共2页
Fine Chemicals
