催化氢化法合成4-乙酰氧基苯乙烯  

Synthesis of 4-Acetoxystyrene via Catalytichydrogenation Method

作　　者：姜晓萍[1] 左翔[1] 蔡烽[1] 杨晖[1] 

机构地区：[1]南京工业大学材料科学与工程学院,江苏南京210009

出　　处：《精细化工》2011年第9期920-923,共4页Fine Chemicals

基　　金：江苏省自然科学基金(BK2007187)~~

摘　　要：以4-羟基苯乙酮为原料,经乙酰化、催化氢化和脱水反应,合成了化合物4-乙酰氧基苯乙烯,总收率为68.5%。用核磁共振氢谱、红外光谱对中间产物以及目标产物进行了结构表征。重点探讨和优化了催化氢化反应的工艺条件。结果表明,以占4-乙酰氧基苯乙酮质量10%的Raney-Ni为催化剂,在反应温度80℃、压力3 MPa、搅拌速度600 r/min、无水乙醇(每克4-乙酰氧基苯乙酮用4 mL无水乙醇)为溶剂的条件下进行催化氢化反应,4-乙酰氧基苯乙醇的收率可达83.1%;脱水反应采用全氟磺酸树脂作催化剂,4-乙酰氧基苯乙烯收率达85.0%。4-Acetoxystyrene （Ⅳ） was synthesized from 4-hydroxyacetphenone （ Ⅰ ） by acetylation, catalytichydrogenation and dehydration with an overall yield of 68.5%. The structure of the intermediate and target products was elucidated by spectrum techniques including Ⅰ HNMR and IR. The catalytiehydrogenation process was optimized, and the optimum conditions were ascertained as follows： reaction temperature 80℃, reaction pressure 3 MPa and stir rate 600 r/min, using Raney-Ni dosage 10% （ based on the weight of 4-acetoxyacetophenone） as the catalyst and 4 mL ethanol （ 1 g 4- acetoxyacetophenone） as the solvent. The yield is 83.1% under the above conditions, while the yield of the dehydration is 85.0% with Nafion-H as catalyst.

关 键 词：4-乙酰氧基苯乙酮 4-乙酰氧基苯乙醇 催化氢化 脱水反应 精细化工中间体 

分 类 号：O621.3[理学—有机化学] O625.12[理学—化学]