9,10-二氰蒽合成方法的改进

以蒽为原料,经溴化和氰化两步合成了光敏剂9,10-二氰蒽(DCA)。从反应溶剂的选择及提纯方法等方面改进了DCA的合成方法,提高了溴化和氰化反应的收率。结果表明,溴化反应时,控制溴的滴加温度为30℃,收率可达95%;合成DCA时,采用连续抽提法提纯,以DMSO为溶剂,反应中生成的无机盐完全溶解,粗产物不经抽提DCA收率可达74%～75%;而选用N-甲基吡咯烷酮为溶剂,DCA可与溴化铜形成配合物CuBr_2·DCA·CuBr_2,此配合物加热易分解,DCA收率达到93%。

IMPROVEMENT OF SYNTHETIC METHOD FOR PHOTOSENSITIZER 9,10-DICYANOANTHRACENE

9,10-Dicyanoanthracene (DCA) was prepared by cyanation of 9,10-Dibromoanthracene, which was synthesized by bromination of anthracene.The synthesis method of DCA was improved ai- ming to raise the yields.Several solvents such as DMSO and N-methylpyrrolidone were used in the step of cyanation and the purification method was modified.The results showed that up to 95% of the 9,10-dibromoanthracene yield could be obtained by controlling the bromine addition temperature at 30℃.Continuous extraction was confirmed to be an efficient method for the purification of impure DCA.When DMSO was used as solvent,in which CuBr_2 can dissolve,the extraction process could be avoided and the yield of DCA reached 74%-75%.Using N-methylpyrrolidone as solvent,a complex of DCA with CuBr_2 formed with the formula of CuBr_2·DCA·CuBr_2.The complex decomposed easi- ly when it is heated,so the yield of DCA can reach 93%.DCA and its complex were identified by ele- ment analysis,IR and UV-Vis.