摘要
以硝基苯为原料,经溴化,脱硝基醚化后制得间溴苯甲醚。将溴酸钾分批加入到硝基苯和硫酸的混合液中,在35.0℃反应4.0 h,过滤,然后用乙醇重结晶得到间溴硝基苯,产率82.8%。将间溴硝基苯溶于环己烷中,并慢慢滴加到已经搅拌反应0.5 h的环己烷,、甲醇、氢氧化钾及四丁基溴化铵的混合液中。升温至60.0℃反应3.5 h,冷却、水洗、盐酸洗、水洗、无水硫酸钠干燥蒸去环己烷就得到间溴苯甲醚,产率为85.6%,纯度为98.9%。
M-bromoanisole was synthesized through bromiation of nitrobenzene, then denitration. The intermediate of m-bromonitrobenzene was synthesized in a yield of 82.8%, via bromation of nitrobenzene for4.0 h at 35.0 ℃, where the bromine was produced by the decomposition of potassium bromate in aqueous sulfuric acid. A solution of 3-bromonitrobenzene in cyclohexane was added to a heterogeneous mixture of cyclohexane, methanol, solid KOH, and tetrabutylammonium chloride, with vigorously stirring, then kept at60.0 ℃ for 3.5 h. The resulting mixture was cooled and washed with water and washed with aq. HCl solution and washed with water. The m-bromoanisole was obtained in a yield of 85.6% and a purity of 98.9%.
出处
《浙江化工》
CAS
2015年第11期9-11,26,共4页
Zhejiang Chemical Industry
关键词
硝基苯
溴化
醚化
间溴苯甲醚
合成
nitrobenzene
bromination
methylation
m-bromoanisole
synthesis
