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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%。
Using 4-hydroxyacetophenone as raw material, the compound 4-acetoxystyrene was synthesized by acetylation, catalytic hydrogenation and dehydration. The total yield was 68.5%. The structures of the intermediates and the target products were characterized by 1H - NMR and IR spectra. The process conditions of catalytic hydrogenation are discussed and optimized. The results showed that at a reaction temperature of 80 ℃, a pressure of 3 MPa, a stirring speed of 600 r / min, anhydrous ethanol (per gram of 4-acetoxy The yield of 4-acetoxyphenethyl alcohol reached 83.1%. The perfluorinated sulfonic acid resin was used as the catalyst in the dehydration reaction. The yield of 4-acetyl The yield of oxystyrene was 85.0%.