2,5-二溴对二甲苯合成条件的研究

Study on synthetic conditions of 2,5-dibromo-P-xylene

[目的]研究制备双光子蛋白质荧光探针的中间产物2,5-二溴对二甲苯的合成条件.[方法]以对二甲苯为原料,在控制物料配比、溶液浓度、反应时间的条件下通过变换紫外线照射与反应温度等因素探索合成2,5-二溴对二甲苯的最适合条件.[结果]紫外线照射可降低反应的重复性,2,5-二溴对二甲苯产率为37.1%±22.7%;在无紫外线照射且避光环境下,0℃,10~15℃,19~24℃及40℃时,2,5-二溴对二甲苯的产率分别为43.60%±3.12%,53.13%±3.79%,50.83%±9.83%,43.23%±6.84%,在10~15℃时2,5-二溴对二甲苯的产率最高（P〈0.05）.[结论]在避光条件下,循环水控制温度为10~15℃是合成2,5-二溴对二甲苯的最适合条件.

OBJECTIVETo study the synthetic conditions of 2,5-dibromo-P-xylene as an intermediator of preparing a series of two-photon protein fluorescent probes.METHODS Under control of concentration of solution,material ratio and reaction time,the optimal synthetic conditions for 2,5-dibromo-P-xylene from P-xylene as the starting material were studied by conversion of irradiating ultraviolet（UV）and changing reaction temperature.RESULTS The UV irradiation caused the reduction of reaction repeatability,and the productive rate of 2,5-dibromo-P-xylene was 37.1% ±22.7%.Under no UV irradiation and away from light,at 0 ℃,10-15 ℃,19-24 ℃,40 ℃,the productive rates of 2,5-dibromo-P-xylene were43.60%±3.12%,53.13% ±3.79%,50.83% ±9.83%,43.23% ± 6.84%,respectively,and the2,5-dibromo-P-xylene yield was the highest at 10-15℃（P〈0.05）.CONCLUSION Away from light and10-15℃ controlled by circulating water are the optimal synthetic conditions of 2,5-dibromo-P-xylene.