间-(三氟甲基)苯甲酸的合成  

Synthesis of m-Trifluoromethylbenzoic Acid

作　　者：彭天成 马德 左识之[3] 荣志忍 薛仲华[3] 

机构地区：[1]上海试四赫维化工有限公司,上海200940 [2]上海工程技术大学,上海200336 [3]华东理工大学化学与制药学院,上海200237

出　　处：《精细化工》2003年第6期371-373,共3页Fine Chemicals

摘　　要：以α,α,α 三氟甲苯(Ⅰ)为原料,合成了间 (三氟甲基)苯甲酸。Ⅰ与三聚甲醛及氯磺酸在n(Ⅰ)∶n(三聚甲醛)∶n(氯磺酸)=1∶1 4∶1 2,反应温度40～50℃下反应3h,制得间 (三氟甲基)氯化苄(Ⅱ),收率为60 3%。在引发剂存在下Ⅱ在65～70℃时通入干燥氯气,反应18h制得三氯产物,收率达92%。使其进一步水解得到产品间 (三氟甲基)苯甲酸,收率达到90%以上。mTrifluoromethylbenzoic acid was prepared from α, α, αtrifluorotoluene(Ⅰ).Ⅰ with 80% H2SO4 reacted with trioxymethylene and chlorosulfonic acid in mole ratio n(Ⅰ)∶n(trioxymethylene)∶n(chlorosulfonic acid)=1∶14∶12 at 40-50 ℃ for 3 h to give 3trifluoromethylbenzyl chloride(Ⅱ) in 603% yield.Then the reaction of Ⅱ with dry chlorine gas and initiator at 65-70 ℃ for 18 h produced 1trichloromethyl3trifluoromethylbenzene in 92% yield.Subsequent hydrolysis produced mtrifluoromethylbenzoic acid in 90% yield and over.

关 键 词：间-(三氟甲基)苯甲酸 氯甲基化 侧链氯化 水解 

分 类 号：TQ245.12[化学工程—有机化工]