4,7-二溴-2,1,3-苯并噻二唑的工艺研究

The Technical Study of 4,7-Dibromo-2,1,3-Dinitrobenzothiadiazole

本论文探究了基于苯并噻二唑的荧光染料中间体4,7-二溴-2,1,3-苯并噻二唑的合成工艺,通过探索液溴比例、反应温度以及时间等多种因素对4,7-二溴-2,1,3-苯并噻二唑产率的影响,得出了最佳反应条件,并发现了一种提纯方法。最佳反应条件为:在47%的氢溴酸中,液溴为3当量,120℃下反应8 h,并用乙酸乙酯进行重结晶方法提纯,此优化条件下,产率可达到91.72%。

In this paper,we have explored the synthesis process of 4,7-dibromo-2,1,3-dibromobenzothiadiazole,which is a fluorescent dye based on benzothiadiazole.By exploring the effects of liquid bromine ratios,reaction temperature and time on the yield of 4,7-dibromobenzothiadiazole,we obtain the best reaction conditions and explore a purification method.The optimum reaction conditions are as follows:47%hydrobromic acid,liquid bromine(3 eq),reaction time and temperature(8 hours at 120℃),and purification is carried out by recrystallization with ethyl acetate.Under these optimum conditions,the yield could reach 91.72%.