The synthesis technique of 2-methyl-6-nitroaniline was studied. In previous method, acetylation and nitration of 2-methylaniline were completed in one pot, but the nitration reaction temperature was difficult to be controled. To improve the method, the acetylation and nitration were detached into two parts. The structure of the product, its by-product and its intermediate were characterized by IR,NMR and MS. The results show that the temperature of nitration process can be controlled easily,and the yield is 59.4% and the purity is up to 99.68%.