摘要
以对氨基苯甲醚、硫氰酸铵为原料在酸催化下制备了对甲氧基苯基硫脲,通过单因素实验方法研究了反应原料的配比、反应时间及反应温度等工艺参数对合成对甲氧基苯基硫脲收率的影响,获得的较佳合成工艺条件为:对氨基苯甲醚5.7g,硫氰酸铵3.1g,盐酸3.3m L,水量8m L,反应温度90℃,反应时间为9h。平行放大实验结果表明,产品的收率大于95%,产品的纯度为99.4%,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对甲氧基苯基硫脲。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。
1-(4-methoxyphenyl)tlalourea was ettectwety prepareo Irom p-anlslome anu ammonium thiocyanate with acidic catalyst. The effects of technical parameters on the yield of 1-(4-methoxyphenyl) thiourea were studied through single-factor experimental method, such as raw materials ratio, reaction time and reaction temperature, etc. The optimal condition was p-anisidine 5.7g, ammonium thiocyanat 3.1g, hydrochloric acid3.3mL, water SmL, reaction temperature 90℃, and reaction time 9h. The results of larger scale experiments proved that the average yield was 95% and the pureness was 99.4%. The FTIR and NMR spectrum suggest that the synthetic compounds was 1-(4-methoxyphenyl)thiourea. The process of this synthesis technology was facile, safe, environment friendly with high product yield and easy production.
出处
《化工进展》
EI
CAS
CSCD
北大核心
2015年第8期3110-3112,3123,共4页
Chemical Industry and Engineering Progress