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一锅法合成3-溴丙基乙酸酯
引用本文:杨晓娜,姜恒,宫红.一锅法合成3-溴丙基乙酸酯[J].化学研究,2008,19(4):48-51.
作者姓名:杨晓娜  姜恒  宫红
作者单位:辽宁石油化工大学,化学与材料科学学院,辽宁,抚顺,113001
摘    要:以1,3-丙二醇、氢溴酸(48%)和冰醋酸为原料,在带水剂的作用下,一锅法合成了3-溴丙基乙酸酯.考察了带水剂及追加醋酸或醋酸酐量对产率的影响,并通过气质联用仪对粗产品进行分析测定,推断其反应机理.结果表明:较适宜的合成条件为1,3-丙二醇0.21mol,1,3-丙二醇与氢溴酸(48%)、冰醋酸摩尔比为1:1:1.3,在带水剂甲苯(21mL)的作用下,反应2.5h,反应结束前1h追加4.8mL醋酸酐,合成效果最好,产率可达到95.7%.

关 键 词:3-溴丙基乙酸酯  气质联用仪  带水剂  一锅法

One-pot Synthesis of 3-Bromopropyl Acetate
YANG Xiao-na,JIANG Heng,GONG Hong.One-pot Synthesis of 3-Bromopropyl Acetate[J].Chemical Research,2008,19(4):48-51.
Authors:YANG Xiao-na  JIANG Heng  GONG Hong
Institution:(College of Chemistry and Materials Science, Liaoning Shihua University, Fushun 113001, Liaoning, China)
Abstract:3-Bromopropyl acetate was synthesized in one pot reaction of trimethylene glycol with an aqueous solution of hydrogen bromide(48 %)and acetic acid(molar ratio,1:1:1.3).The effects of water-carrying agents and the additional quantity of acetic acid or acetic anhydride on the yield were investigated,meanwhile,the crude product was analyzed by GC-MS and the reaction mechanism was proposed.The experimental result showed that the optimal condition was as follows:the molar ratio of trimethylene glycol,hydrogen bromide and acetic acid was 1:1:1.3.When trimethylene glycol was 0.21 mol,refluxed 2.5 h with 21 mL toluene.After 1.5 h,additional 4.8 mL acetic anhydride was added,the yield of 3-bromopropyl acetate was high up to 95.7 %
Keywords:3-bromopropyl acetate  GC/MS  water-carrying agent  one-pot synthesis
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