3,5-二碘水杨酰氯的高效合成工艺

Efficient Synthesis Process of 3,5-Diiodosalicylic Chloride

为提高医药中间体3,5-二碘水杨酰氯在工业生产中的收率和纯度,实现降本增效的同时,使其满足更高的产品指标要求,以3,5-二碘水杨酸为原料,氯化亚砜为酰氯化试剂,选取低沸点的二氯甲烷作溶剂,研究了3,5-二碘水杨酰氯的合成工艺,对该反应的投料比、反应温度和时间等条件进行了优化。FTIR和HPLC分析结果表明,其最佳工艺条件为:55℃回流反应4~5 h,3,5-二碘水杨酸和氯化亚砜的物质的量比为1∶3,减压蒸除溶剂得到最终产品,收率和纯度均可达到99%以上。

In order to improve the yield and purity of the pharmaceutical intermediate 3,5-diiodosalicylic chloride in industrial production,to realize the enhancement of the cost and to meet the higher product index requirements,3,5-diiodide water Salicylic acid was used as the raw material,thionyl chloride was used as the chlorination reagent,and the low-boiling dichloromethane was selected as the solvent to study the synthesis process of 3,5-diiodosalicylic chloride.The reaction conditions such as the feeding ratio,reaction temperature and time were optimized.FTIR and HPLC analysis results show that the best process conditions are:reflux reaction at 55℃for 4~5 hours,the ratio of 3,5-diiodosalicylic acid and thionyl chloride is 1∶3,and vacuum distillation the final product is obtained by removing the solvent,and the yield and purity can reach more than 99%.