中间体O-3-氯-2-丙烯基羟胺的合成研究

Synthesis of Intermediate O-3-chloro-2-propylhydroxylamine

O-3-氯-2-丙烯基羟胺肟法合成的操作简单,反应安全,产品收率高,被广泛应用工业生产。不可避免生成的杂质影响了产品质量和收率,杂质前驱体在醚化反应中产生,对杂质前驱体形成机理进行了合理推测,中间产物N-乙酰基-O-(3-氯-2-丙烯基)羟胺与反式-1,3-二氯丙烯反应生成了三级胺。确定了醚化反应的最佳反应条件减少杂质前驱体生成,使用羟胺水溶液参与反应,在反应温度60℃、投料比n(羟胺):n(NaOH):n(反式-1,3二氯丙烯)=1:2.1:1.0时得最高产品收率87.6%。

The synthesis of O-3-chloro-2-propylhydroxylamine oxime method is simple in operation,safe in reaction and high in product yield,which is widely used in industrial production.The impurity precursors were produced in the etherification reaction,and the formation mechanism of the impurity precursors was reasonably speculated.The intermediate product N-acetyl-O-(3-chloro-2-propenyl)hydroxylamine reacted with trans-1,3-dichloropropene to form tertiary amine.The optimal reaction conditions for the etherification reaction are determined to reduce the generation of impurity precursors.Using hydroxylamine aqueous solution to participate in the reaction,the highest yield of 85.5%was obtained when the reaction temperature of 60℃,the feed ratio is n(hydroxylamine):n(NaOH):n(trans-1,3-dichloropropene)=1:2.1:1.0.