溴代烷烃的清洁合成及表征

Clean Synthesis and Characterization of Bromoalkanes

以工业副产品溴化钾为溴源,水为溶剂,在溴化钾0.1mol,醇0.08mol,浓硫酸5～8mL,水2.5～4.5mL,回流反应4h条件下,合成了12种溴代烷烃,包括直链溴代烷烃、支链溴代烷烃、溴代环烷烃。经折光率、1HNMR、IR、元素分析对其结构进行了表征。水相经生石灰简单处理后,达到环保排放要求。讨论了合成条件对不同结构溴代烷烃收率的影响,考察了该工艺的放大及重复使用稳定性。

Twelve bromoalkanes were synthesized from industrial by-product potassium bromide that the by-product in industry as bromine donator in water, which included linear--chain bromoalkanes, branched--chain bromoalkanes and bromocyclanes. The reaction conditions were as follows： potassium bromide 0.1 mol, alcohol 0.08 mol, concentrated sulfuric acid 5-8 mL, water 2.5--4.5 mL, and refluxed for 4 h. The structures of pure products were characterized by index of refraction, JH NMR, IR and elemental analysis. Aqueous phase simply disposed by calcium oxide can meet the environmental protection requirements. The effect of reaction conditions on the yields were discussed and the magnification and reuse experiments were investigated.