1-溴-4-乙氧基-2,3-二氟苯的合成及性能表征

以2,3-二氟苯乙醚、溴素为原料,还原铁粉为催化剂,合成了1-溴-4-乙氧基-2,3-二氟苯。考察了反应温度、溴素与还原铁粉的物质的量及反应时间对合成反应的影响,确定了最佳工艺条件为:反应温度为-2~-8℃,溴素用量为1.04 mol,还原铁粉用量为0.017 5 mol,反应时间为3 h。最后通过重结晶,得到了含量大于99%的白色晶体状产品,收率为93%。并对产物用GC-MS,IR和DSC进行了表征。

Synthesis and characterization of 1-bromo-4-ethoxy-2,3-difluorobenzene

With the 2,3-difluoroethoxybenzene, the bromine as raw materials and reduced iron powder as catalyst,the 1-bromo-4-ethoxy-2,3-difluorobenzene was synthesized.The influences of reaction temperature,the bromine and reduced iron powder amount of substance and the reaction time on the synthesis reaction were investigated.The optimum process conditions were as follows:reaction temperature is -2～-8 ℃;amount of bromide is 1.04 mol;amount of reduced iron powder is 0.017 5 mol,reaction time is 3 h.At last the white crystalline product which content is more than 99%,is gained by re-crystallization, the yield is 93%,and its structure is characterized by GC-MS,IR and DSC spectra.