3-仲丁基-6-甲基-5-溴脲嘧啶的合成  

Synthesis of 5-Bromo-3-sec.-butyl-6-methyluracil

作　　者：范晓泉[1] 芮必胜[1] 顾浩[1] 黄友林[1] 

机构地区：[1]南京大学化学化工学院,江苏南京210093

出　　处：《精细与专用化学品》2007年第1期11-13,16,共4页Fine and Specialty Chemicals

摘　　要：以仲丁胺和氰酸钾为原料,在85℃下反应2h制得仲丁脲;仲丁脲与乙酰乙酸甲酯在对甲苯磺酸催化下78℃缩合脱水24h得到3-(3-仲丁基)脲-2-丁烯酸甲酯;再与甲醇钠在68℃下环合2h得3-仲丁基-6-甲基脲嘧啶钠盐。用稀盐酸将3-仲丁基-6-甲基脲嘧啶钠盐酸化后得3-仲丁基-6-甲基脲嘧啶,之后与液溴在85℃下反应1h后得目标产品3-仲丁基-6-甲基-5-溴脲嘧啶,总产率为50.52%。中间产物及最终产物用熔点、红外、核磁以及元素分析进行了表征确认。Using sec.-butylamine and potassium cyanate as raw material, sec.-butylurea was prepared at 85℃ for 2 hours. With paratoluenesulfonic acid used as catalyst, sec. -butylurea was condensed with methylacetoacetate for 24 hours at 78℃ to get 2-butenole aeid-3-[[[[ （1-methylpropyl） amino] acrbonyl] amino] methyl ester. Then the product reacted with sodium methoxide at 68℃ for 2 hours to afford sodium 3-sec, -butyl-6-methyluracil. And the 3-sec, -butyl-6-methyluracil was obtained through acidification of solid 3-sec. -butyl-6-methyluracil with dilute hydrochloric acid. Then 3-sec. -butyl-6-methyluracil reacted with bromine at 85℃ for 1 hour to obtain the objective product 5-bromo-3-sec. -butyl-6-methyluracil, the total yield was 50. 52%. Some important intermediates and the final product were characterized and identified by melting point measurement, IR, NMR and elemental analysis.

关 键 词：仲丁胺 氰酸钾 3-仲丁基-6-甲基-5-澳脲嘧啶 除草剂 

分 类 号：TQ457.2[化学工程—农药化工]