4–甲基–2,3,5,6–四氟苯甲醇的合成

化工进展

4–甲基–2,3,5,6–四氟苯甲醇的合成

何明阳，陈圣春，谢英梅，陈群

江苏工业学院，江苏省精细石油化工重点实验室

出版日期:2006-07-25 发布日期:2006-07-25

Synthesis of 4-methyl-2,3,5,6-tetrafluorobenzene methanol

HE Mingyang，CHEN Shengchun，XIE Yingmei，CHEN Qun

Jiangsu Provincial Key Lab. of Fine Petrochemical, Jiangsu Polytechnic University

Online:2006-07-25 Published:2006-07-25

摘要/Abstract

摘要： 以2,3,5,6–四氟对苯二甲醇为起始原料，经氯化、常压催化氢解制得4–甲基–2,3,5,6–四氟苯甲醇。研究表明，在甲苯中用盐酸氯化时，温度为100～105℃、反应6 h、盐酸与2,3,5,6–四氟对苯二甲醇用量物质的量比为1.4，4–甲基–2,3,5,6–四氟苯甲醇产率为96.4%；在甲醇溶剂中以Pd/C为催化剂，温度为50℃、4–氯甲基–2,3,5,6–四氟苯甲醇与10%Pd/C与甲醇质量比为1∶0.05∶9.0，常压氢解4 h，4–甲基–2,3,5,6–四氟苯甲醇产率为99%，两步反应总产率为95.4%。

Abstract: 4-Methyl-2,3,5,6-tetrafluorobenzenemethanol (Ⅲ) was prepared from 2,3,5,6–tetrafluoro–1,4–benzenedimethanol (Ⅰ) by chlorination and hydrogenolysis. In toluene, hydrochloric acid and (Ⅰ) in molar ratio 1.4 reacted at 100～105℃ for 6 h to yield 96.4% of 4–chloromethyl–2,3,5,6–tetrafluorobenzenemethanol (Ⅱ). In methanol, the catalytic hydrogenolysis of (Ⅱ) was carried out at 55℃ for 4 h with the mass ratio of (Ⅱ) to Pd/C catalyst to methanol= 1:0.05:9.0, with the (III) yield of 99%. The overall yield of the two -step synthesis was 95.4%.

何明阳，陈圣春，谢英梅，陈群. 4–甲基–2,3,5,6–四氟苯甲醇的合成 [J]. 化工进展.

HE Mingyang，CHEN Shengchun，XIE Yingmei，CHEN Qun. Synthesis of 4-methyl-2,3,5,6-tetrafluorobenzene methanol[J]. Chemical Industry and Engineering Progree.