对氟苯甲酰氯的合成

Synthesis of p-Fluorobenzoyl Chloride

以对氟甲苯为原料,经光氯化、水解、减压精馏合成对氟苯甲酰氯。对氟甲苯在光照及副反应抑制剂作用下,125-145℃与氯气反应合成对氟三氯甲苯,收率94.8%;水解反应的较优工艺为:120℃,n(水)∶n(对氟三氯甲苯)=0.98∶1.00,对氟苯甲酰氯收率91.5%,总收率86.7%。产品结构经红外光谱、质谱及核磁共振氢谱确认。

p-Fluorobenzoylchloride was synthesized with p-fluorotoluene by photochlorination,hydrolysis and vacuum distillation.In the presence of visible light and side-reaction inhibitor,p-fluorotoluene reacted with chlorine at 125-145 ℃,the yield of p-fluorobenzotrichloride was 94.8%;p-fluorotoluene reacted with water at 120 ℃,the mole ratio of water to p-fluorobenzotrichloride was 0.98∶1,the yield of p-fluorobenzoyl chloride was 91.5%,the total yield of p-fluorobenzoyl chloride was 86.7%.The structure of target product was identified by IR,MS and 1H NMR.