2-Nitrobenzene-1,3-diol was obtained through a series of physical and chemical processes containing sulfonation, nitration, and hydrolysis etc. and treated with dimethyl sulfate to give an anti-UV intermediate. It has been shown by investigating various technologic conditions mentioned above that resorcinol can be completely two-sulfonated and finally resulting in 2-nitrobenzene-1,3-diol with yield of 63.5% and contents over 99.7% when 20% oleum used as sulfonation reagents and 1,3-dimethoxy-2-nitrobenzene can also be obtained with 75.6% by treating 2-nitrobenzene-1,3-diol with dimethyl sulfate at 80 ℃ for 4 h as the molar ratio of dimethyl sulfate to 2-nitrobenzene-1,3-diol is 2.2 : 1.0.