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出 处:《化学与生物工程》2013年第12期53-54,共2页Chemistry & Bioengineering
摘 要:以邻氟苯胺为原料,以亚硫酸氢钠替代常用的二氧化硫作为磺化剂,经重氮化和氯磺化两步反应制备邻氟苯磺酰氯,考察了投料方式和亚硫酸氢钠用量对收率的影响,确定适宜的投料方式为:将亚硫酸氢钠分成A、B两部分,先将A部分加入盐酸中,再将B部分和重氮盐溶液同时滴入含A的混合溶液中;邻氟苯胺和亚硫酸氢钠的适宜摩尔比为1∶2。该工艺步骤少、操作简单、对环境友好、对设备要求低,总收率高达84.3%。2-Fluorobenzenesulfonyl chloride had been synthesized by diazotization and chloro-sulfonation of 2-fluoroaniline using sodium hydrogen sulfite as sulfonating reagent instead of the conventional sulfur dioxide.And effects of feeding method and sodium hydrogen sulfite amount on the yield were investigated.The optimum feeding method was as follows:sodium hydrogen sulfite was divided into two parts,part A was added into hydrochloric acid,part B and the diazonium salt solution were gradually added into the mixture solution containing A,the optimum n(2-fluoroaniline) ∶ n(sodium hydrogen sulfite) was 1 ∶ 2.The process had few steps and simple operation with a total yield as high as 84.3 %,which was environmental friendly.
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