酸酐(Ⅰ)催化氧化合成晶体2-巯基吡啶-N-氧化物钠盐研究  

Study on Catalytic Oxidation Preparation of Crystals of 2-mercaptopyridine-N-oxide Sodium

作　　者：张珍明[1] 王丽[1] 李树安[1] 耿平兰[1] 

机构地区：[1]淮海工学院化学工程系,江苏连云港222005

出　　处：《淮海工学院学报（自然科学版）》2006年第4期35-37,共3页Journal of Huaihai Institute of Technology:Natural Sciences Edition

基　　金：江苏省高校高新技术产业化发展项目(JHB05-50)

摘　　要：研究了以蒽和顺丁烯二酸酐的加成物酸酐（I）为催化剂，催化过氧化氲氧化2-氯吡啶再与硫氢化钠反应合成2-巯基吡啶-N-氧化物钠盐的方法。在2．5h内将质量分数509，5的过氧化氢54g，在60-65℃下滴入57g2-氯吡啶、13g酸酐（I）和20mL乙酸的混合物中，继续反应3h，用水萃取生成的产物，与100g25％硫氢化钠水溶液反应得到晶体2-巯基吡啶-N-氧化物钠盐晶体，收率63.7％。另外还研究了反应温度、时间和催化剂套用次数对催化氧化反应的影响。The preparation of 2-mercaptopyridine-N-oxide sodium was studied with anhydride （ I ） as the catalyst. The product was obtained by Diels-Alder reaction of anthracene and maleic anhydride, and the catalytic oxidation of 2-chloropyridine with H2O2, which then reacted with NariS. According to the method, 54 g of H2O2 （50%） was added dropwise to the mixture of 57 g 2-chloropyridine and 13 g anhydride and 20 mL acetic acid at 60-65℃ for 2. 5 h, and the reaction was extended for 3 more hours. The product was extracted with water, and reacted with Naris to give 2 mercaptopyridine-N-oxide sodium with the yield rate of 63. 7%. The effect of oxidation temperature, time and runs of catalyst reused on the yield of 2-chloropyridine-N-oxide was also discussed.

关 键 词：2-巯基吡啶-N-氧化物钠盐 2-氯吡啶 酸酐 催化氧化 晶体制备 

分 类 号：TQ252.2[化学工程—有机化工]