氧氯化法制备5-氯-8-羟基喹哪啶的研究

Study on the Preparation of 5-chloro-8-hydroxyquinaldine with Oxidative Chlorination

研究了以8-羟基喹哪啶、过氧化氢为主要原料，通过氧氯化方法制备医药和农药的重要中间体5-氯-8-羟基喹哪啶的工艺条件.8-羟基喹哪啶、过氧化氢和质量分数为30％的盐酸投料物质的量比为1：1．05：16．7，在10～15℃下把过氧化氢滴加到8-羟基喹哪啶和盐酸的混合物中反应2h，抽滤分离出5-氯-8-羟基喹哪啶盐酸盐，用质量分数30％盐酸萃取，用质量分数为28％的氨水中和至PH=6．7得到5-氯-8-羟基喹哪啶，质量分数大于99％，收率为74．7％。研究了投料比、反应温度和时间对5-氯-8-羟基喹哪啶收率的影响。

5-chloro-8-hydroxyquinaldine, an important intermediate used for medicine and agriculture, was prepared by oxidative chlorination of 8-hydroxyquinaldine with H2O2. The optimal conditions are as follows： the molar ratio of 8-hydroxyquinaldine ： H2O2 ：HCl（30%） = 1： 1.05： 16.7, and H2 O2 added dropwise to the mixture of 8-hydroxyquinaldine and hydrochloric acid at 10 -15 ℃ for 4 h. After working up, 5-chloro-8-hydroxyquinaldine was obtained with the yield rate of 74. 7% and the purity rate of 99%. The effect of ratio of raw materials, reaction temperature and time on the yield of 5-chloro-8-hydroxyquinaldine was also investigated.