6-氯鸟嘌呤合成工艺的改进

Improved Technology of the Synthesis of 6-Chloroguanine

以鸟嘌呤为起始原料,首先鸟嘌呤与N,N-二甲基甲酰胺和三氯氧磷反应,其后调节溶液pH值在3-4范围内进行水解反应,制得2-甲酰氨基-6-氯嘌呤,再经碱水解、中和得6-氯鸟嘌呤。考察了投料方式、重结晶溶剂对收率的影响,得到适宜的工艺条件为：投料时,先将三氯氧磷在低温下滴入N,N-二甲基甲酰胺配成混合溶液,其后滴入鸟嘌呤,在1,2-二氯乙烷中进行反应;重结晶溶剂选用N,N-二甲基甲酰胺,产品收率达78%（以鸟嘌呤计）,纯度为99%。

2-Formylamino-6-chloropurine was synthesized through the reaction of guanine with N,N-dimethylformamide and phosphorus oxychloride,then hydrolyzed under condition of pH 3—4,and through alkaline hydrolysis,neutralization to produce 6-chloroguanine.Factors influencing the reaction yield were studied,such as feeding mode and solvents for recrystallization.The optimum technical condition： phosphorus oxychloride is added dropwise to N,N-dimethylformamide at low temperature to prepare a mixing solution,then the mixing solution is dropped to the solution of 1,2-dichloroethane dissolving guanine,solvents for recrystallization is N,N-dimethylformamide.The total yield reached 78%（based on guanine） and the purity is 99%.