摘要
以邻(对)硝基氯苯、氢氧化钠和甲醇为原料,以苄基三甲基溴化铵为相转移催化剂,氧气作为氧化剂,在高压釜中合成邻(对)硝基苯甲醚,考察了相转移催化剂、氧化剂种类、甲醇浓度、反应时间对硝基氯苯醚化反应的影响。结果表明,在n(苄基三甲基溴化铵)∶n(邻硝基氯苯)∶n(氢氧化钠)=0.3∶1.0∶1.1,m(无水甲醇)∶m(硝基氯苯)=2.0∶1.0,通入氧气至压力为0.1 MPa,反应温度110℃,反应时间2 h的条件下,硝基氯苯转化率和硝基苯甲醚选择性均>99.5%。
o/p-nitroanisole was synthesized in an autoclave using o/p-nitrochlorobenzene, sodium hydroxide and methanol as raw materials, benzyltrimethylammonium bromide as phase transfer catalyst, oxygen as oxidant. The effects of phase transfer catalyst, oxidant type, methanol concentration and reaction time on etherification of nitrochlorobenzene were investigated. The results showed that under the conditions of n(benzyltrimethylammonium bromide)∶n(p-nitrochlorobenzene)∶n(NaOH) = 0.3∶1.0∶1.1, m(anhydrous methanol)∶m(nitrochlorobenzene)=2.0∶1.0, oxygen up to 0.1 MPa, a reaction temperature of 110 ℃ and a reaction time of 2 h, the conversion of nitrochlorobenzene and selectivity of nitroanisole both reached above 99.5%.
作者
唐晓婵
付永丰
夏雪强
高修正
岳涛
Tang Xiaochan;Fu Yongfeng;Xia Xueqiang;Gao Xiuzheng;Yue Tao(Shandong Chemical Industry Research Institute,Organic Reaction in Aqueous Engineering Research Center of Shandong Province,Qingdao University of Science&Technology,Jinan,Shandong 250014,China)
出处
《化学世界》
CAS
2023年第1期42-46,共5页
Chemical World
基金
山东省“泰山学者”建设工程基金(No.08190201)资助项目。
关键词
硝基氯苯
硝基苯甲醚
甲醇
氢氧化钠
高压法
甲醚化
nitrochlorobenzene
nitroanisole
methanol
sodium hydroxide
high pressure method
methyl etherification
