熔融晶析法合成对硝基苯甲酰氯  

A NOVEL SYNTHESIS AND PURIFICATION OF P-NITROBENZOYL CHLORIDE

作　　者：申东升[1] 林原斌[1] 

机构地区：[1]湘潭大学化学系

出　　处：《湘潭大学自然科学学报》1994年第3期58-62,共5页Natural Science Journal of Xiangtan University

摘　　要：本文研究了在溶剂存在下，以三氯化磷—氯气为酰氯化试剂、以溶融晶析提纯法合成对硝基苯甲酰氯的工艺过程，考察了各反应因素与产率之间的关系．发现当三氯化磷、底物重量比为４５：５０，反应温度为５０～６０℃，反应时间为２ｈ时。产率达９９．２％．找到了一种综合指标都较好的晶析熔剂，经熔融晶析提纯的酰氯产品．含量达９８．５％以上．对产品进行了红外谱、热分析谱和高效液相色谱测定．This paper introduces the synthesis and purification of para-nitrobenzoy chloride (1). The preparation of I by reacting p-nitrobenzoic acid with phosphorus pentachloride or dichloride sulfoxide, and the purification of I by distillation under diminished pressures have long been known and are widely described in the literature.These methods of purifying and synthesizing I, however,are objectionable on account of the difficulties in highly vacuum distill,tion and in handling phosphoruus pentachloride.In this paper a process for the synthesis of I comprises the treatment of p-nitrobenzoic acid with phasphorus trichlorlde and chlorine in the presence of a suitable solvent such as carbon tetrachloride for 2 h at 50-60℃ to give I in 99. 2% yield. It has been reported that the purification of I has been achieved by distilling off the solvent used in the reaction and the phosphorus oxychloride formed in the reaction, and then by pouring this melting leaves as residue into the solvent, and then by cooling, followed by filtrating this solvent with separation of I as the solid with 98. 5% purfity. IR, DSC, MP, and HPLC data were obtained.The advantage of this modification is. the increase in yield and purify of I, and,what is more, the avoidance of highly vacuum distillation.

关 键 词：对硝基苯甲酰氯 芳香酸 酰氯化 熔融晶析法 

分 类 号：TQ246.12[化学工程—有机化工]