| 周海波,钱阳,张新慧,丁浩,陈天云.化学通报,2015,78(10):945-948. |
| 一锅法合成间羟基苯甲醛工艺研究 |
| One-pot Syntheses Of m-Hydroxybenzaldehyde |
| 投稿时间：2015-01-19 修订日期：2015-03-30 |
| DOI： |
| 中文关键词: 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 |
| 英文关键词:m-hydroxybenzaldehyde m-nitrobenzaldehyde stannous chloride dehydrate one-pot synthesis reduction diazo-reaction hydrolysis |
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| 中文摘要: |
| 以间硝基苯甲醛为原料,采用“一锅法”合成技术经过氯化亚锡还原、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、亚硝酸钠用参数对产物收率的影响。实验结果表明,一锅法合成间羟基苯甲醛的最佳合成工艺是,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90min、重氮化时间75min、亚硝酸钠为1.4g时,间羟基苯甲醛总收率达到76.5%。红外光谱和核磁共振谱测试的结果表明所合成的化合物为间羟基苯甲醛。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。 |
| 英文摘要: |
| In this paper, one-pot syntheses process of m-hydroxybenzaldehydevia successive reduction, diazo-reaction, hydrolysis reactions with m-nitrobenzaldehyde as raw materialwas studied. 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 the optimized conditions of one-pot syntheses of m-hydroxybenzaldehyde were as follows: n(m-nitrobenzaldehyde): n(stannous chloride dehydrate)=1:3, reduction temperature 90℃, reduction time 90min,diazo-reaction time 75min., sodium nitrite 1.40g. Under these conditions, the total yield of m-hydroxybenzaldehyde was 76.5%. The FTIR and NMR spectrum suggest that the synthetic compounds was m-hydroxybenzaldehyde. The process of the synthesis technology was facile, safe , environment friendly, high product yield and easy production. |
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