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出 处:《化学工程师》2013年第3期68-70,共3页Chemical Engineer
摘 要:本文主要研究了从邻氟苯胺为原料,经过乙酰化、磺酰化、氨解、脱乙酰基、氯取代,脱磺酰胺基得到氯美昔布中间体2-氯-6-氟苯胺。本文还研究了邻氟乙酰苯胺制备的工艺条件,确定最佳反应时间为1h,最佳料液比为1∶1.25。3-氟-4-乙酰氨基苯磺酰氯制备的最佳用量摩尔之比为1∶4.5。产品经核磁共振谱及红外光谱分析,确定为目标化合物。在最佳反应条件下,产品总收率为29.8%。This thesis is mainly a detailed introduction of the process for preparing 2-chloro-6-fluoroben- zenamine using 2-fluorobenzenamine as material, through acetylation, sulfonylation, ammonolysis, deacetylation, chlorine displacement, desulfonamide to obtain the intermediate of Lumiracoxib. This paper also studied the 2-flu- oroacetanilide preparation process conditions through single-factor-experiments. The best condition was found: re- action time was 1 hour, the best material liquid ratio of 1:1.25. The optimum amount of molar ratio was at 1:4.5 in preparing 4-acetamido-3-fluorobenzene-l-sulfonyl chloride. The structure of target compound was confirmed by the analysis of H-NMR, IR. Under the optimal reaction conditions, the total yield of product was 29.8%.
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