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作 者:孙会 李岳 SUN Hui;LI Yue(Zhejiang Huafang Pharmaceutical Co.,Ltd.,Huangyan,Zhejiang 318020;Dongchang Industry Co.,Ltd.,Linhai,Zhejiang 317000)
机构地区:[1]浙江华方药业股份有限公司,浙江黄岩318020 [2]东昌工业(临海)有限公司,浙江临海317000
出 处:《化工生产与技术》2021年第4期8-10,I0002,I0003,共5页Chemical Production and Technology
摘 要:针对2-氨基丁酰胺盐酸盐现有合成工艺操作复杂、副反应多,分离、纯化困难,废盐多、总收率低的问题,采用氰化钠为原料与氨气反应,进行氨解、再同丙醛缩合,水解,成盐制得2-氨基丁酰胺盐酸盐的合成方法,进行了氨解、水解反应工艺参数的对比实验。结果表明,氨解反应,氨气的质量分数大于30%,氨气与氰化钠的摩尔配比大于3时,30℃下反应2 h,得到2-氨基丁腈,收率98.1%;水解反应,丙酮与2-氨基丁腈的摩尔比0.75时,10℃以下反应2 h,得到2-氨基丁酰胺,收率94.8%。总收率达到93%,2-氨基丁酰胺盐酸盐质量分数达到99%。该方法具有操作简单、转化率高、收率高、杂质低、三废少等特点,是一种有利于工业化生产的合成新方法。Aiming at the problems of complex operation,more side reactions,difficult separation and purification,more waste salt and low total yield of 2-aminobutyramide hydrochloride,sodium cyanide was used as raw material to react with ammonia,ammonolysis,condensation with propanal,hydrolysis and salt formation to prepare 2-aminobutyramide hydrochloride.The results showed that 2-aminobutyronitrile was obtained with the yield of 98.1%when the mass fraction of ammonia was greater than 30%,the molar ratio of ammonia to sodium cyanide was greater than 3,and the reaction was carried out at 30℃for 2 h.Hydrolysis reaction,acetone and 2-aminobutyronitrile molar ratio 0.75,under 10℃for 2 h,2-aminobutyramide,the yield of 94.8%.The total yield reached 93%,and the mass fraction of 2-aminobutyramide hydrochloride reached 99%.This method has the advantages of simple operation,high conversion rate,high yield,low impurity and less waste.It is a new synthesis method for industrial production.
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