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研究了以蒽和顺丁烯二酸酐的加成物酸酐(Ⅰ)为催化剂,催化过氧化氢氧化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2.5 h内将质量分数50%的过氧化氢54 g,在60~65℃下滴入57 g 2-氯吡啶、13 g酸酐(Ⅰ)和20 mL乙酸的混合物中,继续反应3 h,用水萃取生成的产物,与100 g 25%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。
A method was developed for the synthesis of 2-mercaptopyridine-N-oxide sodium salt by the reaction of 2-chloropyridine with hydrogen peroxide and then with sodium hydrosulfide using the addition of anhydride of anthracene and maleic anhydride as catalyst. In 2.5 h mass fraction of 50% hydrogen peroxide 54 g, at 60 ~ 65 ° C was added dropwise 57 g of 2-chloropyridine, 13 g of anhydride (Ⅰ) and 20 mL of acetic acid mixture, the reaction was continued for 3 h, The resulting product was extracted with water and reacted with 100 g of 25% sodium hydrosulfide aqueous solution to give crystalline sodium pyrithione-N-oxide crystals in 63.7% yield. In addition, the effects of reaction temperature, time and number of catalyst application on the catalytic oxidation reaction were also studied.