Synthesis of 2-Amino-4,6-dimethoxypyrimidine(ADM)
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摘要
Using malononitrile as the raw material, a novel synthesis route of 2-amino-4,6-dimethoxypyrimidine(ADM) was put forward, in order to solve the instability in first step reaction of industrial synthesis. The influence of reactant ratio, temperature and time on product quality and yield was explored. The results showed that ADM was successfully prepared through acetyl chloride route, the yield was higher than that of industrial production process, and the process stability was good, with the product purity over 99%. Therefore, the new synthesis route is suitable for industrial production.
Using malononitrile as the raw material, a novel synthesis route of 2-amino-4,6-dimethoxypyrimidine(ADM) was put forward, in order to solve the instability in first step reaction of industrial synthesis. The influence of reactant ratio, temperature and time on product quality and yield was explored. The results showed that ADM was successfully prepared through acetyl chloride route, the yield was higher than that of industrial production process, and the process stability was good, with the product purity over 99%. Therefore, the new synthesis route is suitable for industrial production.
Using malononitrile as the raw material, a novel synthesis route of 2-amino-4,6-dimethoxypyrimidine(ADM) was put forward, in order to solve the instability in first step reaction of industrial synthesis. The influence of reactant ratio, temperature and time on product quality and yield was explored. The results showed that ADM was successfully prepared through acetyl chloride route, the yield was higher than that of industrial production process, and the process stability was good, with the product purity over 99%. Therefore, the new synthesis route is suitable for industrial production.
引文
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[2]LIU JH.Synthesis of 3,4-dihydropyrimidin-2(1H)-one derivatives using sulfonic salicylic acid as catalyst[J].Contemporary Chemical Industry,2008,37(1):56-62.(in Chinese).
[3]ZHENG W,YATES SR,PAPIERNIK SK.Transformation kinetics and mechanism of the sulfonylurea herbicides pyrazosulfuron ethyl and halosulfuron methyl in aqueous solutions[J].Journal of Agricultural and Food Chemistry,2008,56(16):7367-7372.
[4]DENG F,HATZIOS KK.Characterization of cytochrome P450-mediated bensulfuron-methyl o-demethylation in rice[J].Pesticide Biochemistry and Physiology,2002,74(2):102-115.
[5]ZHU PH.Synthesis of 2-chloro-4,6-dimethoxypyrimidine[J].Contemporary Chemical Industry,2005,34(5):330-331.(in Chinese).
[6]HUANG J,SONG JR,REN YH,et al.Preparation,crystal structure and theoretical calculation of 4,6-dimethoxy-2-(methoxycarbamidothiocarbamido)pyrimidine[J].Acta Chimica Sinica,2006,64(1):9-16.(in Chinese).
[7]WANG DX,BAI ZS.A collection of new pesticides[M].Wuhan:Central China Normal University Press,1998:31.(in Chinese).
[8]ROUCHAUD J,NEUS O,CALLENS D,et al.Soil metabolism of the herbicide rimsulfuron under laboratory and field conditions[J].Journal of Agricultural and Food Chemistry,1997,45(8):3283-3291.
[9]ZHANG DB,REN YH,DU DH,et al.Crystal structure,theoretical calculation and bioactivity of 1-(4-methoxylbenzoyl)-3-(4,6-dimethylpyrimidin-2-yl)thiourea[J].Acta Chimica Sinica,2008,66(21):2409-2415.(in Chinese).
[10]XIONG Z.Study on synthetic process of2-amino-4,6-dimethoxypyrimidine[D].Nanjing:Southeast University,2013.(in Chinese).
[11]PARIKH KS,VYAS SP.Synthesis and spectral studies of some novel Schiff base derived with pyrimidines[J].Journal of Chemical and Pharmaceutical Research,2012,4(4):2109-2111.
[12]FUCHS JJ.Propenimidates:U.S.Patent,4,235,802[P].1980-11-25.
[13]LACHHEIN S.Process for the preparation of aminopyrimidines:U.S.Patent 4,831,138[P].1989-5-16.