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在微波辐射下,以甲基磺酸为溶剂,由氯代间苯二酚和氯代邻苯二甲酸酐快速合成含氯荧光素,通过正交实验确定了最优化实验条件:微波辐射时间为80 s,微波功率为560 W,反应物的物质的量比2.3∶1,产率73%。产物的结构经过IR、1HNMR、MS、元素分析等表征。通过对含氯荧光素的荧光光谱性质的研究,发现该类化合物最大荧光发射光波长在512～550 nm范围内,且随着氯原子个数的增加,最大发射波长明显红移。
Under microwave irradiation, chlorofluorescein was rapidly synthesized from chlorinated resorcinol and chlorophthalic anhydride by using methylsulfonic acid as solvent, and the optimum experimental conditions were determined by orthogonal experiments: the microwave irradiation time was 80 s, the microwave power was 560 W, the ratio of the reactants was 2.3: 1 and the yield was 73%. The structure of the product was characterized by IR, 1HNMR, MS, elemental analysis. The fluorescence spectra of chlorofluorescein were studied. The maximum fluorescence emission wavelength of this kind of compounds was found to be in the range of 512-550 nm. With the increase of the number of chlorine atoms, the maximum emission wavelength was significantly red-shifted.