The synthesis of 3 chloro 2 nitrotoluene using 2,6 dichloroaniline as starting material by diazotization, substitution, condensation, decarboxylic reaction was studied and the best conditions of the synthetic proc...The synthesis of 3 chloro 2 nitrotoluene using 2,6 dichloroaniline as starting material by diazotization, substitution, condensation, decarboxylic reaction was studied and the best conditions of the synthetic procedures were confirmed. Dichloronitrobenzene was obtained in 78.9% yield based on 2,6 dichloroaniline. The reaction of 2,6 dichloronitrobenzene and methyl cyanoacetate with potassium carbonate catalyst in N,N dimethyl formamide gave methyl 2 cyano 2 (3′ chloro 2′ nitrophenyl) acetate in 80.2% yield. The third procedure product 3 chloro 2 nitrophenylacetic acid was obtained by hydrolysis in 82.6% yield. Decarboxylation reaction of 3 chloro 2 nitrophenylacetic acid produced 3 chloro 2 nitrotoluene in 72.9% yield.The structure of products was identified by IR and NMR.展开更多
As a good antimicrobial active ingredient, 2,4,4′ trichloro 2′ hydroxydiphenyl ether has been already commercially available since 1970s. For this paper halogenated hydroxydiphenyl ethers were prepared and purifi...As a good antimicrobial active ingredient, 2,4,4′ trichloro 2′ hydroxydiphenyl ether has been already commercially available since 1970s. For this paper halogenated hydroxydiphenyl ethers were prepared and purified, and their analytical conditions by HPLC were studied. Further purification of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was also studied. The adsorption ability of different decolourants, e.g. alumina and bentonite, for each component in crude product of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was varied. 2,4,4′ trichloro 2′ hydroxydiphenyl ether might be adsorbed by active carbon. The colored impurities might be adsorbed by alumina. The colorless impurities might be adsorbed by bentonite.展开更多
文摘The synthesis of 3 chloro 2 nitrotoluene using 2,6 dichloroaniline as starting material by diazotization, substitution, condensation, decarboxylic reaction was studied and the best conditions of the synthetic procedures were confirmed. Dichloronitrobenzene was obtained in 78.9% yield based on 2,6 dichloroaniline. The reaction of 2,6 dichloronitrobenzene and methyl cyanoacetate with potassium carbonate catalyst in N,N dimethyl formamide gave methyl 2 cyano 2 (3′ chloro 2′ nitrophenyl) acetate in 80.2% yield. The third procedure product 3 chloro 2 nitrophenylacetic acid was obtained by hydrolysis in 82.6% yield. Decarboxylation reaction of 3 chloro 2 nitrophenylacetic acid produced 3 chloro 2 nitrotoluene in 72.9% yield.The structure of products was identified by IR and NMR.
文摘As a good antimicrobial active ingredient, 2,4,4′ trichloro 2′ hydroxydiphenyl ether has been already commercially available since 1970s. For this paper halogenated hydroxydiphenyl ethers were prepared and purified, and their analytical conditions by HPLC were studied. Further purification of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was also studied. The adsorption ability of different decolourants, e.g. alumina and bentonite, for each component in crude product of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was varied. 2,4,4′ trichloro 2′ hydroxydiphenyl ether might be adsorbed by active carbon. The colored impurities might be adsorbed by alumina. The colorless impurities might be adsorbed by bentonite.
