6-溴-2-溴甲基-5-羟基-1-甲基吲哚-3-羧酸乙酯的合成工艺研究

Research on 6-bromo-2-bromomethyl-5-hydroxy-1-methyl-indole3-carboxylic acid ethyl ester synthesis technology

采用5-乙酰氧基-1,2-二甲基吲哚-3-羧酸乙酯和溴素为原料,于四氯化碳中,在过氧化苯甲酰催化下,合成6-溴-2-溴甲基-5-羟基-1-甲基吲哚-3-羧酸乙酯,HPLC进行跟踪检测。采用正交设计研究确定了最佳合成工艺参数为:物料比1为n(5-乙酰氧基-1,2-二甲基吲哚-3-羧酸乙酯)∶n(四氯化碳)=1∶18.3,物料比2为n(5-乙酰氧基-1,2-二甲基吲哚-3-羧酸乙酯)∶n(溴素)=1∶2.84,反应时间5 h,反应温度45℃。在最佳条件下收率为84.6%,纯度为98%以上,达到了优化的目的。

Using 5-acetyl-1,2-dimethylindole-3-carboxylate, bromine as the raw material, the carbon tet- rachloride, 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-dim- ethyl-indole-3-carboxylic acid ethyl） ： n （CTC） = 1：18.3, the ratio of materials 2 for n （5-acetyl-1,2-dim- ethyl-indol-3-carboxylic acid ethyl ester） ：n（bromine） = 1：2.84 ,reaction time 5 h,reaction temperature is 45 ~C. Under optimum conditions a yield of 84.6% ,and the purity of more than 98% ,to achieve the purpose of optimization.