Huang Bi-rong
2013
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Journal
Applied Chemical Industry
Abstract
Using 5-acetyl-1,2-dimethylindole-3-carboxylate,bromine as the raw material,the carbon tetrachloride,the benzoyl peroxide catalytic synthesized and subjected to HPLC tracing detection of 6-bromo-2-bromomethyl-5-hydroxy-1-methyl-indole-3-carboxylic acid ethyl ester.Using the orthogonal design study to determine the optimal synthesis of process parameters:the ratio of materials 1 for n(5-acetoxy-1,2-dimethyl-indole-3-carboxylic acid ethyl) ∶ n(CTC)=1 ∶ 18.3,the ratio of materials 2 for n(5-acetyl-1,2-dimethyl-indol-3-carboxylic acid ethyl ester) ∶ n(bromine)=1 ∶ 2.84,reaction time 5 h,reaction temperature is 45 ℃.Under optimum conditions a yield of 84.6%,and the purity of more than 98%,to achieve the purpose of optimization.