第 45 卷第 6 期Vol. 45 No. 6
2015 年 12 月Dec 2015

所属栏目:农药及中间体

反马氏加成法合成1-溴代正辛烷
丁宗旺,李斌栋* (南京理工大学 化工学院,江苏 南京 210094)
摘 要:无溶剂条件下,在自由基引发剂的作用下,溴化氢气体以鼓泡的方式通入到反应体系中,与1-辛烯(1-octene)发生反马氏加成,得到目标产物1-溴代正辛烷。考察了引发剂的种类、 溶剂、反应温度、反应时间、投料比和反应前活化温度等对收率的影响。结果表明,以过氧化苯甲酰(BPO)作引发剂、反应温度20℃、反应1.5 h、n(1-辛烯)∶n(溴化氢)=1.0∶1.2、无溶剂条件下,产品收率大于80%,蒸馏后纯度大于99%。
关键词:反马氏加成反应;1-溴代正辛烷;过氧化苯甲酰
中图分类号:O622.2  文献标识码:A  文章编号:1009-9212(2015)06-0014-04
Synthesis of α-Bromooctane by Anti-Markovnikov Addition Reaction
DING Zong-wang, LI Bin-dong* (College of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China)
Abstract:α-Bromooctane was synthesized from anti-Markovnikov addition reaction of hydrogen bromide flow with 1-octene without the assistant of solvent. Reaction conditions including the type of radical initiators, the amount of solvents, the reaction time and temperature, feed ratio and activation temperature were evaluated. The optimum reaction conditions were as following: benzoyl peroxide(BPO) as initiator, reaction temperature of 20℃, reaction time of 1.5 h, 1.0:1.2 molar ratio of 1-octene to HBr. The typical yield of product is more than 80% with a purity of more than 99% after distillation.
Key words:anti-markovnikov addition reaction; α-bromooctane; benzoyl peroxide
作者简介:丁宗旺(1990-),男,山东菏泽人,硕士研究生,研究方向:精细化工中间体的合成(E-mail:gtarsix04@126.com)。
联 系 人: 李斌栋,教授,研究方向:药物及精细有机中间体的合成。
收稿日期:2015-09-29