2,5-二甲基十二烷基苯同分异构体的精细合成与表征.pdfVIP

石汹学报〈石油加工) 2007 年 6 月 ACTA PETROLEI SINICA (PETROLEUM PROCESSING SECTION) 第 23 卷m3 期 文章自号: 1001-8719(2007) 03-0075-05 2 ， 5-二甲基十二娱基苯同分异构体的 精细合成与表征 2.5-DIMETHYLDODECYLBENZENE ISOMERS 丁伟， 王瑞，于 涛，曲广森，温海飞 DlNG Wei. WANG Rui. YU Tao. QU Guang-miao. WEN Hai-fei {大庆石油学院化学化工学院，黑龙江大庆 163318) ( Chemitryand Chemical Eg;nttring cUegt , Daqing Pttrol.m lnslltult , Daql1fg 163318 , Chtna) 摘要:以对二甲苯为原料， 经 Friedel-Craf l s 融化反应、格氏反应、 Pd/C 还原等步骤合成了 2 . 5-二甲基十二烧:!ili *的6 种问分异构体。通过正交试验斜阳的合成中间体 2.5-二甲基苯~十二烧法扇的最佳工艺条件为 n(~.t 二职 苯) ，圳股氯): n(A IC1 , ) = 3: l 1.1，消力nl张;(时体系温度 15(; ，反应时间 6 h. 在上述条件下得到的 2 ， 5-二甲 基笨幸在卡二统基画面的收率为 68. 8Yo -70. 5Yo. 利用红外光谱与核磁共振氢潜对部分中间体及产物透衍了袭征，确 定了化合物的结构与所设计的分子结构相同. 关键词: 长链多统基苯s 精细合1Ii.. 表征 中图分爽-Ij: TQ24 1. 1 文献标识码: A Abstr.lct , Six isomers of 2 , 5-dimethyldodecylbenzene were synthesized through several stcps , involv ing F ri edel-Crafts reaction , Grignard reaction , reducation(Pd/C) ctc. p -Xylene was used as the raw materia l. The optimized conditions for synth esizing 2 ,5-dimethylphenyl dodecyl ketone screened by an or thogonal experimcntal dcsign method w ere as fo llows: the temperature at whi ch acyl chloride was trickled into system was 15.C . the molar ralio of p -xylene to acyl chlorid e and AICb 10 acyl chloride were 3 : 1 and 1. 1 : 1 respectively , the reaclion ti me was 6 h , under which th e yield o f 2 ,5-dimethylphenyldodecyl ketone was between 68.8% to 70 . 5 % . The Slructure of t he intermediates and final products were characterized by lR and 1 日 NMR , proving t hat the mol ecular structure of p repared sampJe w as the same as that of the