Huang You-lin
2007
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Journal
Fine and Specialty Chemicals
Abstract
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-butenoic acid-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.