催化氢化法合成4-乙酰氧基苯乙烯

Synthesis of 4-Acetoxystyrene via Catalytichydrogenation Method

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.