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作 者:程清蓉[1] 刘志雄[2] 周红[1] 潘志权[1]
机构地区:[1]武汉工程大学化工与制药学院,湖北省新型反应器与绿色化学工艺重点实验室,湖北武汉430074 [2]吉首大学化工学院,湖南吉首416000
出 处:《应用化工》2009年第5期675-677,684,共4页Applied Chemical Industry
摘 要:以去甲氨噻肟酸乙酯(DMAT)为原料,对影响反应收率的反应温度、物料配比、相转移催化剂及其用量、甲基化试剂、反应时间等因素进行了研究。最佳反应条件为:反应温度20℃,NaOH为碱性试剂,DMAT∶NaOH∶(CH3O)2SO3为1∶1.2∶1.2,四丁基碘化铵作相转移催化剂,用量为底物摩尔数的7%,硫酸二甲酯为甲基化试剂,乙醇和四氢呋喃为溶剂,反应时间约为4 h,总收率为79%。2- ( 2-Aminothiazol-4 -yl ) - ( Z ) -2- ( methoxyimino ) acetate was synthesized with ethyl-demethyl- aminothiazolyloximate as raw material. The factors affect the reaction were investigated, including the reaction temperature, reagent proportion, phase transfer catalysts, methylateds, reaction time. The optimum conditions were as follows:tempeture was 20 ℃, the mole ratio of DMAT : NaOH : (CH3O)2SO3 was 1 : 1.2 : 1.2, phase transfer catalyst was CTMAC,methylateds was DMSO,solvents was EtOH and THF, reaction time was 3 h. The yield was 79%.
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