摘要
目的研究3,5-二氯-4-氟三氟甲苯的合成工艺。方法以3,4,5-三氯-三氟甲苯和氟化钾为原料通过相转移催化合成目标产物。结果确定了反应的最佳条件为反应物物质的量比n(3,4,5-三氯-三氟甲苯)∶n(氟化钾)=1∶1.5,催化剂与原料质量比m(PEG-600)∶m(原料)=0.5~0.7∶100,原料与溶剂环丁砜(TMSO2)体积比为1∶3~3.5,190~195℃反应12 h,原料转化率大于87%,收率80%,产品纯度大于98%(质量分数)。结论为工业化生产3,5-二氯-4-氟三氟甲苯提供了依据。
Aim To research the synthesis process of 3,5-dichloro-4-fluoro-trifluoro-toluene.Methods The title compound was synthesized from 3,4,5-dichloro-trifluoro-toluene and KF by phase transfer catalysis.Results Using TMSO2 as solvent,mole ratio n(3,4,5-trichlorobenzotrifluride)∶ n(KF)=1∶ 1.5,weight ratio m(PEG-600)∶ m(3,4,5-trichloro-benzotrifluoride)=0.5~0.7∶ 100,volume ratio V(3,4,5-trichlorobenzotrifluoride): V(TMSO2)=1∶ 3~3.5,stirring for 12h at 190~195℃,the conversion of 3,4,5-trichlorobenzotrifluoride is 87%,the yield is 80%,and the content is more than 98%.Conclusion The process was mild and available for synthesis of 3,5-dichloro-4-fluoro-trifluorotoluene.
出处
《西北大学学报(自然科学版)》
CAS
CSCD
北大核心
2010年第1期81-84,共4页
Journal of Northwest University(Natural Science Edition)
基金
陕西省科学技术研究发展计划基金资助项目(2008K06-04)