Journal of Flow Chemistry ( IF 2.7 ) Pub Date : 2020-05-26 , DOI: 10.1007/s41981-020-00094-6 Yi Jin , Junhui Yang , Xiaoliang Feng , Jie Li , Jianguo Xu , Xiaobin Chen , Shuhua Wang , Yanwen Lv , Jiangang Yu
An efficient procedure of continuous-flow microwave reactor, for oxidative bromination with HBr (hydrogen bromide) -DMSO (dimethyl sulphoxide) in large scale is described herein. The reaction is carried out in a metal-free manner, with the use of water as solvent under microwave irradiation conditions. The productivity of this continuous step attains 60 g/min under the optimal conditions, implying a theoretical productivity of 8.6 kg/day. The reaction mixture is screened by thermal insulation accelerometer to ensure the safe process of this reaction in these conditions. 4-Bromo-3-methylanisole is further reacted with formanilide in the presence of cuprous iodide (CuI) and potassium carbonate (K2CO3) to give 4-methoxy-2-methyldiphenylamine, a common intermediate in fine chemical industry such as dye and paper chemistry, in an isolated yield of 65.2%. with more than 200 g scale.
中文翻译:
使用连续流动微波系统开发HBr-DMSO大规模氧化溴化反应,以随后合成4-甲氧基-2-甲基二苯胺
本文描述了连续流微波反应器用于大规模用HBr(溴化氢)-DMSO(二甲基亚砜)氧化溴化的有效方法。反应在微波辐射条件下以水为溶剂以无金属的方式进行。在最佳条件下,此连续步骤的生产率达到60 g / min,这意味着理论生产率为8.6 kg / day。通过绝热加速度计对反应混合物进行筛选,以确保在这些条件下该反应的安全过程。4-溴-3-甲基苯甲醚在碘化亚铜(CuI)和碳酸钾(K 2 CO 3)得到4-甲氧基-2-甲基二苯胺,这是精细化学工业中的常见中间体,例如染料和造纸化学,分离产率为65.2%。重量超过200克。