一锅法合成间羟基苯甲醛工艺研究  

One-Pot Synthesis of m-Hydroxybenzaldehyde

作　　者：周海波[1] 钱阳[1] 张新慧[1] 丁浩[1] 陈天云[1] 

机构地区：[1]合肥工业大学化学与化工学院,合肥230009

出　　处：《化学通报》2015年第10期945-948,共4页Chemistry

摘　　要：以间硝基苯甲醛为原料,采用"一锅法"经氯化亚锡还原、重氮化、水解制得间羟基苯甲醛,研究了物料摩尔比、还原反应时间、还原反应温度、重氮化时间、亚硝酸钠用量等参数对产物收率的影响。结果表明,在优化工艺条件(间硝基苯甲醛与二水合氯化亚锡的摩尔比为1∶3、还原温度90℃、还原时间90min、重氮化时间75min、亚硝酸钠为1.4g)下,间羟基苯甲醛的收率达到76.5%。产物经红外光谱和核磁共振谱确认。该合成技术工艺过程简单,生产安全,环境友好,产品收率高,易于生产。In this paper,m-hydroxybenzaldehyde was synthesized with m-nitrobenzaldehyde as raw material by one-pot process via successive reduction,diazo-reaction,and hydrolysis reactions. The effects of the molar ratio of raw materials（ n（ m-nitrobenzaldehyde） ： n（ stannous chloride dehydrate））,reduction time,reduction temperature,diazo-reaction time and amount of sodium nitrite on the yield of product were investigated. The results showed that under the optimized conditions of syntheses,i. e. n（ m-nitrobenzaldehyde） ： n（ stannous chloride dehydrate） = 1 ∶ 3,reduction temperature 90℃,reduction time 90 min,diazo-reaction time 75 min and sodium nitrite 1. 40 g,the76. 5% yield of m-hydroxybenzaldehyde could be reached. The products were characterized by FT IR and NMR. This process is facile,safe,environment friendly,high yield and easy production.

关 键 词：间羟基苯甲醛 间硝基苯甲醛 二水合氯化亚锡 一锅法合成 还原 重氮化 水解 

分 类 号：TQ244.1[化学工程—有机化工]