4-乙酰氨基苯亚磺酸合成新工艺研究

陈焕章, 冯雪, 张悦, 孙朝利

现代化工 ›› 2018, Vol. 38 ›› Issue (3) : 187 -191.

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现代化工 ›› 2018, Vol. 38 ›› Issue (3) : 187-191. DOI: 10.16606/j.cnki.issn0253-4320.2018.03.041
科研与开发

4-乙酰氨基苯亚磺酸合成新工艺研究

    陈焕章, 冯雪, 张悦, 孙朝利
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Study on new process for synthesis of para-acetamidobenzenesulfinic acid

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摘要

以乙酰苯胺和SO2为原料,一步合成4-乙酰氨基苯亚磺酸。自制了催化效果良好的催化剂,并考察了溶剂种类、溶剂用量、反应温度、反应时间、催化剂用量、通SO2的时间等单因素对产品收率的影响。通过正交实验确定了最佳反应条件,并进行了验证试验。最佳反应条件为:反应温度为60℃、反应时间为6.5 h、通SO2时间为4 h、催化剂质量分数为6.75%、溶剂质量与乙酰苯胺的质量比为7:1。在最佳反应条件下,产品的收率>70%。对目标产物进行了熔点测定、IR、LCMS、HNMR等分析。新工艺反应路线短,原子利用率高,三废量减少,符合绿色化学宗旨,应用前景广阔。

Abstract

para-Acetamidobenzenesulfonic acid is directly synthesized by one-step method using acetanilide and SO2 as starting materials and using high efficient self-prepared catalyst.The effects of solvent species,solvent dosage,reaction temperature,reaction time,catalyst dosage and the time to add SO2 on the product yield are investigated.The product is analyzed by melting point determination,IR,LCMS,HNMR and so on.The optimum reaction conditions are determined by orthogonal experiments,and the verification tests are performed too.The optimum reaction conditions are as follows:reaction temperature is 60℃,reaction time being 6.5 h,time to add SO2 being 4 h,catalyst dosage 6.75% and the mass ratio of solvent to raw materials 7:1.Under the optimum reaction conditions,the product yield exceeds 70%.The new synthetic process has significant advantages,such as short reaction route,high atom utilization rate and fewer wastes and so on,which conforms to the green chemistry aim and has broad application prospect.

关键词

4-乙酰氨基苯亚磺酸 / 新工艺 / 合成 / SO2 / 乙酰苯胺

Key words

p-acetamidobenzenesulfinic acid / new process / synthesis / sulfur dioxide / acetanilide

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4-乙酰氨基苯亚磺酸合成新工艺研究[J]. 现代化工, 2018, 38(3): 187-191 DOI:10.16606/j.cnki.issn0253-4320.2018.03.041

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