Synthesis And Optimization In Coupling Component Of C.I. Disperse Blue 301

Disperse dye is one of the most important types in dye industry. Disperse dyes play a leading role in China. The production of disperse dyes in China is produced mainly by three different companies, that is, Zhejiang Runtu, Zhejiang Longcheng and Zhejiang Jihua. Their productions are all more than 10 million tons. Up to date, the number types of the disperse dyes in have been more than 150, including low-energy type, medium type, high-energy type, the carboxylic acid ester based types, rapid dyeing type, fluorescence type, and so on. China can produce most large-tonnage disperse dyes. The types in disperse dyes with the scale of thousand tons in China are more than 30. And 8 different types of disperse dyes can be produced in the scale of ten thousands tons, that is, Disperse blue H-GL, Disperse blue EX-SF 300%, Disperse yellow brown S-2RFL, Disperse red 3B/FB, Disperse carbuncle S-2GFL, Disperse blue 2BLN, Disperse black EX-SF 300%and Disperse black ECO 300%.3-(N,N-dimethoxyethyl)amino-4-methoxy acetanilide is one of the most important intermediates for disperse dyes, which is the coupling component of top grade disperse dye C. I. disperse blue 301. In the dissertation, we have utilized four synthetic routes to optimize the preparation process, including 1) dimethyl sulfate,2) tosylation (4-methylbenzenesulfonate),3) sodium metholate; and 4) 2-chloroethyl methyl ether. The optimized method was established by the treatment of 3-amino-4-methoxy acetanilide with 2-chloroethyl methyl ether using potassium iodide as catalyst and Na2CO3 as acid trap:n (AMA):n (2-chloroethyl methyl ether)= 1:9 in molar ratio, reaction temperature at 120℃, reaction time for 24 h. Such a synthetic method is with easiness in synthesis and convenience in collecting raw materials. The conversion to the target product is about 94%.