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作 者:彭俊英 李鸣 戴慧 彭东明[1] 王福东[1] 卢茂芳[1] 王瑞嘉 PENG Jun-ying;LIMing;DAI Hui;PENG Dong-ming;WANG Fu-dong;LU Mao-fang;WANG Rui-jia(College of Pharmacy, Hunan University of Chinese Medicine, Changsha 410208, China)
出 处:《精细化工中间体》2018年第2期47-49,共3页Fine Chemical Intermediates
基 金:药学湖南省重点学科开放基金项目[科函(2015)9号-5];湖南省科学技术厅科技计划一般项目(2014SK3024);湖南省"十二五"'药学重点学科(湘教发[2011]76号)
摘 要:以盐酸羟胺和乙酸乙酯为原料,在碱性醇溶液中反应制备乙酰氧肟酸。分别考察反应溶剂、反应温度、反应时间、投料配比和溶剂用量等因素对收率的影响。实验结果表明:在氢氧化钠碱性甲醇溶液中,反应温度为25~30℃、反应时间为5 h、n(盐酸羟胺)∶n(乙酸乙酯)=1.0∶1.2、溶剂用量为乙酸乙酯体积数的4倍时收率达87.2%,纯度达98.3%。Acetohydroxamic acid was synthesized from the reaction of hydroxylamine hydrochloride and ethyl acetate. The affecting factors including the reaction solvents, the ratio of feedstock, the reaction time, the reaction temperature and solvent dosage were investigated. The results showed that the optimal reaction conditions were as following: temperature was 25-30℃; time was 5 h; hydroxylamine hydrochlorid:ethyl acetate was 1.0 ∶1.2; the dosage of slovent was 4 times of ethyl acetate. The product was obtained with a yield of 85.2% with a purity of 98.3%.
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