化工进展2024，Vol.43Issue(12)：6905-6912,8.DOI:10.16085/j.issn.1000-6613.2023-2002
甲酰胺法合成鸟嘌呤工艺
Guanine synthesis process using formamide method
摘要
Abstract
The reduction of 2,4-diamino-5-nitroso-6-hydroxy-pyrimidine(DAHNP)to 2,4,5-triamino-6-hydroxy-pyrimidine(TAHP)and the formation of TAHP sulfate is complicated and involves a large amount of inorganic salts,making it difficult to purify crude guanine(GA).Directly synthesizing GA from DAHNP can not only solve this problem,but also shorten the reaction process and improve the reaction efficiency.Therefore,this article designed a green route for the synthesis of GA by formamide method.This study used methyl cyanoacetate(MC)and guanidine hydrochloride(GH)as raw materials to obtain DAHNP through cyclization and nitrification in one-pot method.The separated DAHNP was then reduced by sodium bisulfite and reacted with formamide dehydration in a closed loop in one-pot to obtain GA.The effects of molar ratio of raw material,dosage of sodium nitrite and mass fraction of sodium methanolate solution on the yield of DAHNP were systemically investigated.The effects of types of reducing agent,dosage and mass fraction of formamide solution on GA yield were studied.When using sodium bisulfite as reducing agent,n(MC)∶n(GH)∶n(CH3ONa)∶n(NaNO2)=1∶1.14∶1.6∶1.2,m(NaHSO3)=3.5g,80%formamide solution and 20%sodium methanolate methanol solution,GA yield could reach 80.7%with purity≥99.0%.The synthesis process was easy to operate and had a simple process,achieving the recovery and utilization of formamide solvent,which was suitable for industrial production.关键词
鸟嘌呤/甲酰胺/氰乙酸甲酯/盐酸胍/一锅法Key words
guanine/formamide/methyl cyanoacetate/guanidine hydrochloride/one-pot method分类
化学化工引用本文复制引用
李彬,刘飞,张天永,姜爽..甲酰胺法合成鸟嘌呤工艺[J].化工进展,2024,43(12):6905-6912,8.基金项目
国家重点研发计划(2022YFB3603101). （2022YFB3603101）
