溴化钾-浓硫酸法合成1-溴代十二烷

Synthesis of 1-bromododecane using potassium bromide-concentrated sulfuric acid method

以工业生产2-羟基-4-正十二烷氧基二苯甲酮的副产品溴化钾为原料,与正十二醇在浓硫酸存在的条件下进行反应合成1-溴代十二烷。通过对反应条件的考察,确定较佳工艺为:溴化钾0.1mol,正十二醇0.08 mol,浓硫酸6 mL,水2.5 mL,回流条件下反应4 h,分离产率高达92.5%。粗产品经气相色谱分析证明几乎无任何副产物,产品经IR和折光率进行表征。

1-Bromododecane was synthesized from potassium bromide which is the by-product of synthesizing 2-hydroxy-4-n-dodecyloxybenzophenone and n-dodecyl alcohol using concentrated sulfuric acid as catalyst. By investigating the reaction condition, the experimental result showed that the optimal conditions are potassium bromide 0. 1 mol, n-dodecyl alcohol 0. 08 mol, concentrated sulfuric acid 6 mL, H2O 2. 5 mI., refluxing for 4 h, the separated yield is high up to 92. 5%. Raw product was analyzed by GC and no by-product was detected almost. Pure product was characterized by IR and index of refraction.